Chemistry Letters · Chemistry Letters Vol.33, No.10 (2004) C-149 Copyright 2004 The Chemical...

Chemistry Lettershttp://www.csj.jp/journals/chem-lett/

Vol.33 No.10 CMLTAGOctober, 2004 ISSN 0366-7022

Copyright 2004 The Chemical Society of Japan

1226 Ligand Influences in Heme–Copper O2-Chemistry as Synthetic Models for Cyto-chrome c Oxidase

O

CuII

O O

CuII

O

FeIII FeIII

µ−η2:η2µ−1,2

O

CuII

O

FeIII

µ−η2:η1

Kenneth D. Karlin and Eunsuk Kim

Recent advances in synthetic modeling of the cytochrome c oxidase heme–copper active site chemistry includes dioxy-gen reactivity studies which lead discrete heme–peroxo–copper assemblies. The coordination and spectroscopic properties(e.g., resonance Raman O–O stretching vibration) are strongly influenced by the copper ligand environment (e.g., ligand den-ticity).

Highlight Review

Letter

1232 Morphological Development and Etching ofGold Thin Film under UV-exposure inChlorine-based Liquids

Liquid with chlorine

Gold

(formation of gold chloride)

hν(UV)

desorption(etch)

reduction to gold Ilsin An and Deokkyeong Seong

C-148 Chemistry Letters Vol.33, No.10 (2004)

Copyright 2004 The Chemical Society of Japan http://www.csj.jp/journals/chem-lett/

1234 Determination of the Field Strengths ofWeak Neutral Ligands Having Oxygen asCoordination Atom

DMSO

DMF MeOH Et2NNO THF

80 60 40 20 0 -20 -40

80 60 40 20 0 -20 -40

4-MePyNO4-ClPyNO

S = 5/2 S = 3/2PyNO

Fe(TPP)L2+

Fe(TiPrP)L2+

δ(ppm)

δ(ppm)

3,5-Me2PyNO

Weakness of oxygen-containingneutral ligands was ranked on thebasis of the pyrrole-H chemicalshifts of the planar [Fe(TPP)L2]+

and highly ruffled [Fe(TiPrP)L2]+

complexes.

Akito Hoshino and Mikio Nakamura

1236 Self-organized Wire-like Aggregates ofPalladium Nanoparticles with Poly(amido-amine)dendrimer

N N

NH

NH

HN

HN

O

O

O

O

N

N

NHHN

O

O

H2N

NH2

NH

NH

O

ONH2

H2N

N

N

HN

HNO

O

HNONH

O

NH2

NH2

H2N

H2N

G1.0 PAMAM dendrimer

Pd(OAc)2

+

500 nmKensuke Naka, Hideaki Itoh, and YoshikiChujo

1238 Highly Active and Selective Pd–Cu–TiO2

Catalyst for the Direct Synthesis of BenzylAcetate by Gas Phase Acetoxylation ofToluene

CH3

AcOH

CH2OAc

++ 1/2 O2 H2O+catalyst

A first report on achieving significantly higher conversionof toluene (ca. 60%) and higher yields of benzyl acetate

Pd−Cu−TiO2 catalyst and successfully overcoming theproblem of catalyst deactivation.

(ca. 55%) through vapor phase acetoxylation usingA. Benhmid, K. V. Narayana, A. Martin,B. Lucke, and M.-M. Pohl

1240 Cobalt-catalyzed Cross-coupling Reaction ofChloropyridines with Grignard Reagents

dioxane

Co(acac)2, RMgX

N RN Cl

R = PhCH2, (CH3)3SiCH2, Ph

Hirohisa Ohmiya, Hideki Yorimitsu, andKoichiro Oshima

1242 VUV Photocatalytic Degradation of Toluenein the Gas Phase

Toluene degraded more fast under 185 nm

(VUV) than that under 254 nm (UV).

0

5

10

15

20

25

30

0 2 864

Inlet concentration (mg/m3)

Rea

ctio

n ra

te (

mg/

m3 .

min

) TiO2/VUVVUVTiO2/UV

Pengyi Zhang, Juan Liu, and Zhongliang Zhang

Chemistry Letters Vol.33, No.10 (2004) C-149


1244 High Electron Drift Mobility in an Amor-phous Film of 2,4,6,-Tris[4-(1-naphthyl)-phenyl]-1,3,5-triazine

N

N N

N2 laser (337 nm)(3.8 × 10−5 V cm−1)

2,4,6-Tris[4-(1-naphthyl)phenyl]-1,3,5-triazine exhibited a high electrondrift mobility of 8.0 × 10−4 cm2 V−1 s−1 in a TOF measurement.

Al

ITO

Tsutomu Ishi-i, Kentaro Yaguma, ThiesThiemann, Masataka Yashima, Kazunori Ueno,and Shuntaro Mataka

1246 Boron Trifluoride Etherate Mediated Dehy-drogenative Nucleophilic Addition Reactionof Aliphatic Ethers in the Presence of AcetalAffording ,-Unsaturated Carbonyl Com-pounds O

R2R1

BF3•OMe2

OR2

R1

Ph R1

OOMeR2

Ph

OMe

Ph

OMe

OMe Ph R1

O

R2 = CH(CH3)R1

BF3•OMe2

- Hydride complex- Proton

Takashi Jobashi, Masaomi Takano, TetsuoHino, Katsuya Maeyama, Keigo Fugami,Hiroyuki Ozaki, Kenji Ogino, and NoriyukiYonezawa

1248 Fabrication of Calcium Carbonate withExquisite Morphologies and Colors througha New Controlled Precipitation Approach

Wei Shan, Bo Wang, Ya-Hong Zhang, Bi-YunWu, and Yi Tang

1250 Direct Observation of Polytungstate Clusterand Monolayer Tungstate on ZirconiumOxide by High-resolution TEM

Direct observation of WO3/ZrO2 by using high-resolution TEM images revealed the

formation of polytungstate cluster with a narrow size distribution ranging in 0.4−0.7 nm, and

the agglomeration into monolayer tungstate after the aging at 1073 K.

Tungstate monolayer

5 nm5 nm

Polytungstate cluster

Atsushi Satsuma, Hitoshi Yokoi, HiroyukiNishiyama, Shiro Kakimoto, Satoshi Sugaya,Takafumi Oshima, and Tadashi Hattori

1252 Novel Anion Exchange Resin-based Catalystfor Liquid-phase Methanol Synthesis at 373–393K

Two model processes, a semi-batch operation and a continuous flow

catalyst performance is sufficiently high.

CO/2H2

Solid catalyst(Cu−Resin-OCH3)

MeOH (liq)

operation for methanol synthesis are possible without recycle if the

Ken-ichi Aika, Hidenobu Kobayashi, KenjiHarada, and Koji Inazu



1254 The Effect of the Si/Al Ratio on the Photolu-minescence Properties of Cu(I)SAPO-5Catalysts

SAPO-5

N2O N2 + O2 N2O

O O O O O O

Si Al P Al P

O OO O O O O O O O

Cu(I)Cu(I)

hν hν

The Cu(I) species characterized by

presence of H2O vapor at 298 K.

the photoluminescenc around490 nm, which is produced by thereduction of Cu(II) ion exchangedwith the bridging hydroxy group(Si−OH−Al) SAPO’sof frameworkwas found to play an importantrole as a stable active site for thephotocatalytic decomposition ofN2O into and even2N 2O in the

at

Haijun Chen, Masaya Matsuoka, JinlongZhang, and Masakazu Anpo

1256 Hybridization of Surface-modified Semicon-ductor Nanoparticles and a Resin

CdSe nanoparticle capped by SH-PMMA polymers (prepared by RAFT technique)

CdSeCdSe

: TOPO : SH-PMMA

Kazuaki Matsumoto, Ryotaro Tsuji, YoshiharuYonemushi, and Tatsushi Yoshida

1258 Synthesis of the Sterically Fixed BiliverdinDerivative Bearing the Z-anti C/D-RingComponent

+

NHMe

Me

O

Ts

NH

CO2tBu

Cl

CO2Allyl

OHC

N

CO2H

N

MeMe

O HNMe

HN

MeO

CO2H

A

BC

D

D

C

HN

MeO Sp-Tol

Ts

A

HNMe

CHO

CO2Allyl

tBuO2CB

Zanti

+

Mostafa A. S. Hammam, Yasue Murata, HidekiKinoshita, and Katsuhiko Inomata

1260 Formation of Surface Nano-step Structuresand Improvement of Photocatalytic Activ-ities of NaTaO3 by Doping of Alkaline EarthMetal Ions

Doping ofSr2+ ions

Formation of nano-step structuresand fine particles!!

Non-doped NaTaO3 Sr-doped NaTaO3

1 µm 0.1 µm

The strategy of improvement of photocatalytic activity Water splitting onNiO (0.2 wt %)/NaTaO3:Sr (2%)using a 400-W high pressureHg-lampH2: 9.5 mmol h–1

O2: 4.7 mmol h–1

Akihide Iwase, Hideki Kato, Hiroaki Okutomi,and Akihiko Kudo

1262 Spongiacysteine, a Novel Cysteine Derivativefrom Marine Sponge Spongia sp.

O

N

CO2H

S

OHOH

H

spongiacysteine

• Isolated from Japanese sponge Spongia sp.• Antimicrobial activity

Keiko Kobayashi, Hiroki Shimogawa, AkiraSakakura, Toshiaki Teruya, Kiyotake Suenaga,and Hideo Kigoshi



1264 Self-assembly of Tetramethylated Resorcin-[4]arene to Form Molecular Capsules Incor-porating Methanol, Ethanol, and Imidazole:A Comparison with the Unsubstituted Resor-cin[4]arene System

Katsuyuki Aoki, Toshiki Nagae, Rei Matsubara,and Ikuhide Fujisawa

1266 Amorphous Molecular Materials with HighCarrier Mobilities: Thiophene- and Seleno-phene-Containing Tris(oligoarylenyl)amines X

XX

N

X

XX

N

X = S : TTPAX = Se : TSePA

X = S : TPTPAX = Se : TPSePA

Hitoshi Ohishi, Masatake Tanaka, HiroshiKageyama, and Yasuhiko Shirota

1268 Color Changes Dependent on the AnisotropicIntercalation of Poly(diacetylenecarboxy-lates) in LDH Clay Hybrids

OOO

O

OOOOOOO

O

LDH LDH

mono-[16,1] mono-[10,11]

Toshio Itoh, Tetsuya Shichi, Tatsuto Yui,Hiroki Takahashi, and Katsuhiko Takagi

1270 Self-assembly of a Novel ManganiferousCoordination Polymer with Mixed Ligands A novel coordination polymer, [(NA)(ONA)Mn(II)] n

(HNA = nicotinic 2H ONA = 2-hydroxyni-acid;

cotinic acid) has been hydrothermally synthesized.It up ofmade mixed-ligands and hexa-is

Mn(II)coordinated linkers. ONA groups bridge Mnions, the right- and left-handed helicaltorisegiving[(ONA)Mn]n chains. The helical are furtherchainsheld groups to form a novel 3-DNAbytogether

chain labeled in cyan color.framework. showsThe diagram one right-handedYouwei Yao, Qiang Cai, Huizhong Kou,

Hengde Li, Dan Wang, Ranbo Yu, Yunfa Chen,and Xianran Xing

1272 One-pot Solution-phase Synthesis of Para-magnetic Co2P Nanorods

A solution-phase route has been developed for the synthesis of cobalt phosphide nanorods. Themicroscope analysis reveals that the nanorods have width of about 10 nm and length of 200−300 nm,which exhibit paramagnetic behavior down to 2 K.

Hongwei Hou, Qing Yang, Chenrong Tan,Guangbin Ji, Benxi Gu, and Yi Xie



1274 Insulinomimetic Vanadyl–Hydroxythiazole-thione Complexes with VO(S2O2) Coordina-tion Mode: The Correlation between the Ac-tivity and Hammett’s Substituent Constant

N

SS

OR

N

SS

OR

V

O

VO(S2O2)Akira Katoh, Mika Yamaguchi, Ryota Saito,Yusuke Adachi, and Hiromu Sakurai

1276 New Approach for the Recovery of BisphenolA fromWater Using Inclusion Complex withQuinoline Derivatives

1.0 M HCl (4.0 mL)

4(1.1 mmol)

OHHON

host-guestcomplexation

3 was recovered in 87% yieldfrom the water solution

Bisphenol A (3) Quinoline (4)

0.1 M NaOH (45.0 mL)

3(1.0 mmol)

inclusion crystal of 3 with 4

Bunpei Hatano, Akiko Aikawa, HideyukiTagaya, and Hiroki Takahashi

1278 Microwave Assisted Facile One-Pot Synthe-sis of 188Re-Complex Using a Tetrahydrobo-rate Exchange Resin. A Bifunctional Chelat-ing Agent for Radiopharmaceuticals HN

SS

NH

3

Na188ReO4, BER, SnCl2 • 2H2O

MWI, 5 min, 300 W

N

SS

N

Re

O

188

5

H

Sang Hyun Park, Hui Jeong Gwon, and KyungBae Park

1280 Palladium-Catalyzed Mizoroki–Heck-typeReactions Using Telluronium Salts

RR

+

Pd(II) catAgOAc

CH3CN, 50 °CTe+Me2I-

X : H, 4-Me, 4-MeO, 4-CF3, 2-Me, 2-MeO R : CO2Bu, CN, CHO, COMe, Ph

X X

Kazunori Hirabayashi, Yoshiko Nara, ToshioShimizu, and Nobumasa Kamigata

1282 A Novel Layered Structure of a New Cadmi-um Chlorophosphate with an ImidazoliumTemplate

Wei Liu, Hao-Hong Chen, Xin-Xin Yang,Man-Rong Li, Ming-Hui Ge, and Jing-Tai Zhao



1284 Growth of Mesoscale Tubular CdS Crystalsvia a Hydrothermal Method

Tubular structure CdS with the range of 0.5−2 mm

3−6 µm in the wall thickness, were successfully

hydrothermal method at 350 ˚C.

in in10−20 µmlength, the external diameter and

grown in sodium hydroxide solution via a

c

Xinzheng Liu and Fan Guo

1286 Preparation of Mixed-metal PolynuclearComplexes by Stepwise Phosphine-bridgingReaction

PdCl

Cl P

P

PdP

P ClCl

Pt

4-Cltp

P4-Cltp

PRh

PClCl

RhP Cl Cl2Cl-

P

P

4-Cltp

PPdP

(BF4)

PdP

Cl P

P PdP

P P

ClPt

4-Cltp

P4-Cltp

P2

(BF4)2

[Rh2Cl4Cp*2]

trans-[PtCl2(NCPh)2]

Sen-ichi Aizawa, Tatsuya Kawamoto, andKenji Saito

1288 Selective Production of "-Caprolactam viaLiquid-phase Beckmann Rearrangement ofCyclohexanone Oxime over HUSY Catalyst

ε-Caprolactam was selectively producedthrough the liquid-phase Beckmannrearrangement of cyclohexanone oximeover HUSY catalyst when the by-productsformation was effectively retarded byblockage of the corresponding activecenters of pre-adsorbed water andbenzonitrile molecules.

NOH

NH

O

H2O-HUSY

in PhCN

Cyclohexanoneoxime

ε -Caprolactam 97% selectivity

Chawalit Ngamcharussrivichai, Peng Wu, andTakashi Tatsumi

1290 Delocalization of Positive and NegativeCharge Carriers on Oligo- and Poly-fluo-renes Studied by Low-Temperature MatrixIsolation Technique

Oligofluorenes with well-defined chain length (n = 1–5) have been synthesized by step-by-stepSuzuki coupling reaction. The spectroscopy of radical anions and cations indicates the clearrelationship between the transition energy and the chain length without saturation in the degree ofdelocalization of excess electrons or holes.

Yoshiko Koizumi, Shu Seki, Anjali Acharya,Akinori Saeki, and Seiichi Tagawa

1292 Direct Observation of Hydroxyapatite Nucle-ation from Amorphous Phase in a Stoichio-metric Calcium/Phosphate Aqueous Solu-tion

In the BF image (left), the morphology of the individual particles is spherical (shape of ACP),not of rod-like shape (HAp crystals). However, the DF image (right) shows many tiny brightspots, which is the evidence of the presence of tiny crystals. Nuclei of the HAp crystals seemto be nucleated directly from ACP and they will develop to rod-like or acicular shapes later.

Sujin Kim, Hyun-Seung Ryu, Hyunho Shin,Hyun Suk Jung, and Kug Sun Hong



1294 A Single-source Approach to MetastableNi3S4 Crystallites and Their Optical Proper-ties NiCl2 + 2 NaS2CNEt2 → Ni(S2CNEt2)2 + 2NaCl

Ni3S4

Xiangying Chen, Zhenghua Wang, XiongWang, Junxi Wan, Jianwei Liu, and Yitai Qian

1296 Synthesizing Multidentate Ferrocenylphos-phines: A Powerful Route to Dissymmetri-cally Tri-Substituted Ferrocenes. X-rayStructure and 13CNMR of a Diaryl–Alkyl-phosphino Ferrocene

The new mixed diaryl/alkyl triphosphine1,2-bis(diphenylphosphino)-1'-(diisopropylphosphino)-4-tert-butylferrocene, Fc(P)2

tBu(PiPr).

Fe P(1)

CNT(1)

CNT(2)

P(2)

P(3)

C(5)

C(14)

C(13)

Jean-Cyrille Hierso, Vladimir V. Ivanov,Regine Amardeil, Philippe Richard, andPhilippe Meunier

1298 Double Elimination Protocol for Access toPyridine-Containing Arylene–Ethynylenes

NOHCN

C6H13

SO(=NTs)Ph

SO(=NTs)Ph

+

NN N

N

C6H13

C6H13

Akihiro Orita, Takehiko Nakano, TaisakuYokoyama, Govindarajulu Babu, and JunzoOtera

1300 A Novel Au12 Supramolecule Composed ofTwo-, Three-, and Four-coordinated Au(I)Centers Constructed on the S3 Scaffolding

Keiko Nunokawa, Tetsuya Sunahara, SatoruOnaka, Kazuya Okazaki, Hiroyuki Imai,Katsuya Inoue, and Tomoji Ozeki

1302 Characteristics of Pyrimidine Nucleobasesthrough Inter-base Interactions on the Crys-tals of the Ternary Copper(II) Complexes

Intermolecular Triple Hydrogen Bonding Interaction

Koichiro Jitsukawa, Mamoru Mizutani,Hidekazu Arii, Ichiro Kubo, Yasuyuki Izu,Tomohiro Ozawa, and Hideki Masuda



1304 Stereoselective Preparation of -Hydroxy-carboxamide by Manganese Complex Cata-lyzed Hydration of,-Unsaturated Carbox-amide with Molecular Oxygen and Phenylsi-lane

PhSiH3

O2 (1 atm)5 mol% Mn(dpm)3

diastereoselectivity

O

Xc*

OHR

O

Xc*R

NXc* =Favored

Disfavored

90 97%

Mitsuo Sato, Yasuhiko Gunji, Taketo Ikeno,and Tohru Yamada

1306 Oxidative Desulfurization of Diesel Oil withHydrogen Peroxide in the Presence of AcidCatalyst in Diesel Oil/Acetic Acid BiphasicSystem

H2O2

acid cat.SR R

SR R

SR R

O

SR RO

[Oil phase]

[AcOH phase]+

OKazumasa Yazu, Mitsunori Makino, and KojiUkegawa

1308 Solvent-free Imino-Aldol Three-componentCouplings on a Conveniently-prepared andReusable Phosphoric Acid-Silica Gel Sup-port

HN

R3 R4

O

R5H3PO4-SiO2

Ar, −5 oC, 16 h

R1

R2

R1CHO + R2NH2

R3

R4

OSiMe3

R5

Sandra Lock, Norikazu Miyoshi, and MakotoWada

1310 Identification of Reaction Model of PyrolysisReaction of HDPE

t/t 0.9

0.0 0.2 0.4 0.6 0.8 1.0

Co

nve

rsio

n

0.0

0.2

0.4

0.6

0.8

1.0

718K723K728K733K

1310

6 5

11

412 9

8 3

7 2

1

Seungdo Kim, Young-Chun Kim, and Eun-SukJang

1312 Single-crystal-to-Single-crystal Polymeriza-tion of 4,40-ButadiynedibenzylammoniumDisorbate UV

X-Rayγ-Ray

Toru Odani, Shuji Okada, Chizuko Kabuto,Tatsumi Kimura, Hiro Matsuda, AkikazuMatsumoto, and Hachiro Nakanishi



1314 Microwave-assisted Synthesis of Single-crystalline CuO Nanoleaves

500 nm500 nm

Single-crystalline CuO nanoleaves with anaverage thickness of about 10 nm and withlateral sizes of hundreds of nanometers toseveral micrometers have been successfullysynthesized by microwave-heating of anaqueous solution containing copper saltand sodium hydroxide.

Zhen-Hua Liang and Ying-Jie Zhu

1316 Iridium-Catalyzed Addition Reactions ofEthynylsilane to Quinolines and Isoquino-lines Activated by Acyl Chloride

N

R1R3

N

R1R2

R4

R4

R3

H TMS

ClCO2Ph or ClCOPh

[IrCl(COD)]2(1~5 mol%)

N

CO2Ph TMS

R3 R1

N

R2

R1

COPh

TMS

R4

R4

R3

2,6-Lutidine

THF, 24 h

R2R2

Yusuke Yamazaki, Ken-ichi Fujita, and RyoheiYamaguchi

1318 ZnO Particles Encapsulated in Porous Cu2ONanoparticle Layer Prepared by UV Light-Induced Photoreduction of Cu(NO3)2.3H2Oover ZnO in Methanol Suspension (111)

(110)

(200)

40 41 42 43 44 45

30 40 50 60

Cu2O/ZnO

ZnO

Inte

nsity

/ a.

u.

2 thetaLianhai Lu and Roland A. Fischer

1320 Synthesis and Characterization of Monodis-perse ZnS Nanospheres

200 250 300 350 400 450 500 550 600 650 7000

100

200

300

400

500

600

700

800

900

1000

1100

Inte

nsity

/a.u

.

Wavelengh/nm

EX EM

------ annealed ZnS

Yue Zhang, Qing Peng, XunWang, and YadongLi

1322 A Study on the Electronic Effect of Reactionsof -Allylpalladiums Using 2-Arylsulfonyl-oxy-3-chloropropenes with Ethyl Malonateand Their Synthetic Utilization

H

H

OCl

O2S X

H

H

ONu

O2S X

Nucleoplile

Pd(0)

MeO>Me>Cl,Br>NO2

rate orderKohei Gotoh, Yasutaka Matsuura, FuminoriHatanaka, Setsuko Sato, Shinzoh Kagabu, andMitsuhiro Yoshimatsu



1324 A Novel One-pot Synthesis of CyanohydrinAlkyl Ethers from Aldehydes Catalyzed byIron(III) Chloride

OR'

R CNRCHO

TMSCNR'OTMS

R = Aryl, Alkyl; R' = Benzyl, Allyl, Alkyl (1o, 2o)

cat. FeCl3

up to 98%

Katsuyuki Iwanami and Takeshi Oriyama

1326 Facile Route for the Preparation of HollowSilica Using Aromatic Desilylation in Phenyl-silsesquioxane Particles

Seung Hoon Han, Tae Sung Si, and Sang ManKoo

1328 Frontier Electron Density Pattern of DioxinCongeners

HOMO of 2,3,7,8-tetrachlorinated dibenzo-p-dioxin.Yoshihiro Mizukami

1330 Pt-implanted Boron-doped DiamondElectrodes for Electrochemical Oxidation ofHydrogen Peroxide

Comparison of Pt-implanted BDD and Pt metal shows much larger signal to background ratio forthe electrochemical oxidation of hydrogen peroxide at Pt-implanted BDD.

Tribidasari A. Ivandini, Rika Sato, YoshihiroMakide, Akira Fujishima, and Yasuaki Einaga

1332 Microwave-assisted Synthesis of Flower-like ZnO Nanosheet Aggregates in a Room-temperature Ionic Liquid

A fast and environmentally benign microwave-assisted route has been developed forsynthesis of flower-like ZnO nanosheets aggregates in ionic liquids. This method may beextended to synthesize other oxides nanomaterials.

a b

Jieming Cao, Jun Wang, Baoqing Fang, XinChang, Mingbo Zheng, and Haiyan Wang



1334 High-Pressure Synthesis and Properties of aCerium Germanide CeGe3 with the CubicCu3Au Type Structure

Ce

Ge

CeGe3

0

50

100

150

0 100 200 300Temperature / K

ρ /

µΩ

cm

Hiroshi Fukuoka and Shoji Yamanaka

1336 Novel Families of Hole-TransportingMonomers and Polymers

O

N

O

NAr NN

Ar NN

NN

HO OH

S S S* *n

SHHS S

(C2H5)3N

Vytautas Getautis, Juozas Vidas Grazulevicius,Tadas Malinauskas, Vygintas Jankauskas, ZbigTokarski, and Nusrallah Jubran

1338 Simple Route for Synthesis of PbS DendriticNanostructured Materials

Novel PbS dendritic nanostructured materials aresynthesized using 2-aminoethanethiol (AET) via simplehydrothermal approach. The morphology evolution ofPbSrod-shapednanostructures is well illustrated and explained in termsof the adsorption of AET molecule on the crystalsurface.

one-dimensionalnanodots,zero-dimensionalfromdendriticthree-dimensionaltostructure

Qing Huang and Lian Gao

1340 A New Approach for the Au/Ag Alloy Nano-particle Formation through the Reduction ofAg(I) to Ag(0) by Amine and IntermetallicElectron Transfer from Ag(0) to Gold(I)Complex

AgI

Growth stage

AuI

NEt3

Intrametallicelectron transfer

Alloy nanoparticles

[Au(C13H27CO2)(PPh3)] +

C13H27CO2Ag

NEt 3

20 nm

Au0

Ag0

Ag0 reductionMari Yamamoto and Masami Nakamoto

1342 An Efficient Catalyst for Low TemperatureSolid-phase Cyclization of Poly(o-hydroxy-amide)

An quantitative solid-phase cyclization of poly(o-hydroxyamide) into poly(benzoxazole) has beendemonstrated using an acid catalyst (5-propylsulfonyloxyimino-5H-thiophen-2-ylidene)-2-(methylphenyl)acetonitrile (PTMA) at 250 °C in 10 min.

HN

HN

OHHO

OCF3F3C PTMA

PHA PBO

ON

O

NCF3F3C

nn

250 °C, < 10 minO O O

Fumihiro Toyokawa, Ken-ichi Fukukawa, YujiShibasaki, and Mitsuru Ueda



1344 Preparation Method Allowing Self-isolationof CdS Nanocrystals Emitting IntenseBand-gap Luminescence

Susumu Kuwabata, Keiko Ueda-Sarson, andTsukasa Torimoto

1346 Large Scale Synthesis of Carbon HollowSpheres from Metal Zinc Powder andEthanol

A simple method was used to prepare carbon hollowspheres with average size of about 400 nm in diameterfrom metal zinc powder and ethanol. The FE-SEM andTEM images show that these carbon spheres have aball-like and vessel-like morphology, all of which havesmooth surfaces and a quite uniform diameter.

Wu Zhang, Jianwei Liu, Zhen Huang, DekunMa, Jianbo Liang, and Yitai Qian

1348 Construction of Z-scheme Type Heterogene-ous Photocatalysis Systems for Water Split-ting into H2 and O2 under Visible LightIrradiation

H2-Photocatalyst

Fe2+

Fe3+

O2-Photocatalyst

Electron relayFe3+/Fe2+ couple

BiVO4 (BG: 2.4 eV)Rh-doped SrTiO3

(Energy gap: 2.4 eV)

Donor level(Rh3+)

O2, H+

H2O

Visible light

CB

VBh+

H+

H2Pt

h+

CB

VB

Visible light

e–

e–

Hideki Kato, Mikihiro Hori, Ryoko Konta,Yoshiki Shimodaira, and Akihiko Kudo

1350 Preparation of "-Caprolactam via Beck-mann Rearrangement of CyclohexanoneOxime: A Mild and Recyclable Process

N N SO2ClCF3SO3

ionic liquid

NOH

N

O

ionic liquid

ScCO2 + CHCl3

(CH2)n

1. n = 3, 2. n = 4

Kun Qiao, Youquan Deng, Chiaki Yokoyama,Hikaru Sato, and Miki Yamashina

1352 Synthesis of Controllable Crystalline Nano-TiO2 at Low Temperature Controllable crystalline nano-TiO2

with high surface area wassuccessfully synthesized at lowtemperature with reversemicroemulsion method by simplyvarying the proportion of Cl– andSO4

2– in aqueous phase ofmicroemulsion. The mechanism offorming different contents ofanatase is proposed. Thephotocatalytic activity of thesamples shows that anatase andrutile have a synergistic effect inenhancing the photocatalyticactivity of TiO2.

Maocheng Yan, Feng Chen, and Jinlong Zhang



1354 A New Class of Substrates for the Nucleo-philic 5-endo-trigCyclization, 1-Trifluorome-thylvinyl Compounds: Syntheses of Indolineand Pyrrolidine Derivatives

N

CF3

N

CF2

N

CF3

or"5-endo -trig "

–

Ts Ts Ts

Junji Ichikawa, Takashi Mori, and Yu Iwai

1356 Iron-Catalyzed Dechlorination of ArylChlorides

ClR

BuMgCl (3 equiv.)10 mol% FeCl3

THF, 50 °CH

R

R = electron-donating group high yield

Haiqing Guo, Ken-ichiro Kanno, and TamotsuTakahashi

1358 The Influence of Polytypic Structures on theSolid-state 13CNMR Spectra of n-Alkanes Mon

Orth II

Intensity

40 30 20 1013C Chemical Shift /ppm

32°C

CH3

inner-CH2

18 16 14

Orth II:15.2 ppmMon:15.5 ppm

The difference in solid-state 13C NMR spectra between the two polytypic structures of n-C36H74

Hideki Kubota, Fumitoshi Kaneko, ChikayoAkita, and Tatsuya Kawaguchi

1360 Allylimidazolium Halides as Novel RoomTemperature Ionic Liquids

Introduction of allyl group onto imidazolium salts improvedviscosity, thermal property and ionic conductivity of thesalts containing halide anion.

Tomonobu Mizumo, Edy Marwanta, NoriyoshiMatsumi, and Hiroyuki Ohno

1362 An Efficient Method for the Ether FormingReaction between Alkyl Diphenylphosphi-nate and Alkoxytrimethylsilane by the Pro-motion of Trimethylsilyl Triflate

Ph2POR R'OTMS ROR'TMSOTf

O

Yohei Kobashi, Tomofumi Minowa, andTeruaki Mukaiyama



1364 Addition of Organostannanes to IsocyanateCatalyzed by a Rhodium Complex

OCNR1 +R1

O

HN R2R2 SnBu3

cat Rh(I)PhOH

THF, 70 °C

Tooru Koike, Masabumi Takahashi, NobumichiArai, and Atsunori Mori

1366 Fabrication of Novel Vanadium DioxideNanorods as CathodeMaterial for Recharge-able Lithium Batteries

VO2(B) nanorods in diameter of40–60 nm and in length up to1–2 µm were fabricated via asurfactant-assisted hydrothermalmethod. Electrochemical test resultsdemonstrate that the nanorodsshow an initial discharge specificcapacity of 306 and 245 mAh/g inthe fifteenth cycle.

Wen Chen, Junfeng Peng, Liqiang Mai, HuaYu, and Yanyuan Qi

1368 Preparation of Protected Nanoparticlesof Bismuth Telluride by Laser Ablation inSolution

Norihisa Watanabe, Jun Kawamata, and NaokiToshima

1370 One-pot Synthetic Method of Allyl Sulfides:Samarium-induced Allyl Bromide MediatedReduction of Alkyl Thiocyanates and DiarylDisulfides in Methanolic Medium

RSCNSm/Allyl bromide/ MeOH

rt, 30min

ArSSAr ArSCH2CH=CH2

RSCH2CH=CH2

Sm/Allyl bromide/ MeOH

rt, 30min Yield: 76% 83%

Yield: 80% 93%

Zhuang-Ping Zhan and Kai Lang

1372 Ab initio Studies on Synthetic Routes of Gly-cine from Simple Molecules via Ammonoly-sis of Acetolactone: Applications of theScaled Hypersphere Search Method

New synthetic routes of glycine have been discovered by theoretical search of ab initio potential energy surfaces. One stepreaction of acetolactone with ammonia can produce glycine without byproducts, and its activation energy is 1.6 kcal•mol-1.Acetolactone can be produced from either carbon dioxide and singlet methylene (CO2 + CH2) or carbon monoxide andformaldehyde (CO + HCHO) with respective activation energies of 3.2 and 36.3 kcal•mol-1.

acetolactone

C

O

C O

Glycine

CO2 + CH2

CO + HCHO C

O

C

ON

+ NH3

Satoshi Maeda and Koichi Ohno



1374 Synthesis and Electrochemical Properties ofSingle-crystal CdV2O6 Nanowire Arrays

Single-crystal cadmium vanadate (CdV2O6)

with that of bulk CdV2O6.

nanowire arrays with the average diameterof 100 nm and length of up to 20 µm werefabricated by a hydrothermal process at140 °C Electrochemicalfor 12 h. testshows that these nanowire arrays deliver arelatively large discharge capacity of90 mA vs at 0.1 mAmetalLi−1gh −2cm(voltage comparedV)3.2−2.0ofwindowXiangying Chen, Xiong Wang, Zhenghua

Wang, Junxi Wan, Jianwei Liu, and Yitai Qian

1376 Synthesis and Luminescent Properties of aNew Twisted Copolymer Containing Phenyl-enevinylene and Spirobifluorene OHC

CHO

t-BuOK

THF

OC4H9

C4H9On+

OC4H9

OC4H9

P(OC2H5)2

(C2H5O)2P OO

Bing Huang, Jun Li, Pin Shao, Jingui Qin,Zuoquan Jiang, Gui Yu, and Yunqi Liu

1378 Zn/CeCl3.7H2O-TBPB: A New and ‘Green’Promoter System for Rapid and Regioselec-tive Thiolyzation of 1,2-Epoxides with ArylDisulfides

O

R

ArSSArZn / CeCl3. 7H2O-TBPB

70 °C

ArS

OH

OH

or SAr

R R

+

Ahmad R. Khosropour, Mohammad M.Khodaei, and Kazem Ghozati

1380 Photochromism of a Diarylethene Trimer ina Bulk Amorphous Phase

MeMe

N

S

S

S

Me

Me

MeMe

Me

Me

S

Me

S

S

N

S

S

S

Me

Me

Me

Me

Me

SF2

F2

F2

F2

S

S

F2F2

F2 F2

F2

Me

MeMe

Me

hν

hν '

F2

F2

F2

F2

F2F2

F2 F2

F2

Arisa Tomari, Tadatsugu Yamaguchi, NaotakaSakamoto, Yuji Fujita, and Masahiro Irie

1382 Crystallization Process of TiO2 Nanopar-ticles in an Acidic Solution

300 400 500 600

A RAR

tpep

=24 h

tpep

=10 min

th/c

=24 h

th/c

=10 min

Inte

nsity

(arb

.uni

t)

Raman shift (cm−1)

Addition of nitric acid at 30 °C to hydrolysis and condensation (h/c)product for peptization yields anatase from amorphous phaseas early as 10 min of peptization (tpep = 10 min) as seen in the Ramanspectrum. However, the anatase formed under such condition has alocally distorted atomic arrangement, as confirmed by a broad bandbetween 425 and 605 cm-1 and shift from the position of anatase (A:515 cm-1). Such a metastable anatase would be prone to dissolve asthermodynamically stable Ti(OH)2

2+ reported in the literature, which, inturn, would crystallize to rutile, which is the eventual phase by thepeptization in this work. The activation energy of the new two-stepprocess at 30 °C has certainly been greatly lowered from a solid-statereaction as the latter requires about 400−1200 °C for directanatase/rutile conversion.Hyunho Shin, Hyun Suk Jung, Kug Sun Hong,

and Jung-Kun Lee



1384 Synthesis and Characterization of BariumSulfate Nanotubes

Tubular barium sulfate, havingdiameters in the range of 200–350 nmand length up to 30 microns, wasfabricated by a nanochannel reactor.The process is very simple, efficient,and easy to control, which can be usedto prepare a wide range of tubularinorganic nanomaterials.

Xiao-Jing Lu, Xian-Wen Wei, Jian Sun,Yong-Hong Ni, Guang-Chao Zhao, and Yin Ye

1386 Redox-controlled Luminescence of a Cyclo-metalated Dinuclear Platinum ComplexBridged with Pyridine-2-thiolate Ions

Pt2

Pt1

Tamami Koshiyama, Ai Omura, and MasakoKato

1388 Synthesis of Li[Ni1=3Co1=3Mn1=3]O2zFz viaCoprecipitation

DSC traces of theLi[Ni1/3Co1/3Mn1/3]O2-zFz at 4.6 V

150 200 250 300 350

Li[Ni1/3

Co1/3

Mn1/3

]O2-z

Fz

[z = 0.15]

626 J g-1

[z = 0.1]

839.2 J g-1

[z = 0.05]

1733 J g-1

[z = 0]

4227 J g -1

Hea

t flo

w /

W g

-1

Temperature / °C

DSC traces of theLi[Ni1/3Co1/3Mn1/3]O2-zFz at 4.6 V

150 200 250 300 350

Li[Ni1/3

Co1/3

Mn1/3

]O2-z

Fz

[z = 0.15]

626 J g-1

[z = 0.1]

839.2 J g-1

[z = 0.05]

1733 J g-1

[z = 0]

4227 J g -1

Hea

t flo

w /

W g

-1

Temperature / °CSeung-Taek Myung, Gil-Ho Kim, and Yang-Kook Sun

1390 Microwave-assisted Synthesis of Nanocrys-talline Metal Sulfides Using an Ionic Liquid

Nanoparticles of metal sulfides (ZnS andCdS) have been successfully synthesizedusing an ionic liquid 1-n-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4)under microwave heating at 100 °C for 10min.

20nm 20nm

Ya Jiang and Ying-Jie Zhu

1392 A Naphthalimide Fluorescent Sensor forZn2þ Based on Photo-induced ElectronTransfer

A new Zn2+ fluorescent sensor exhibits intense fluorescence after complexation with Zn2+ (innanomolar) under physiological conditions. Other cations such as such as Na +, K+, Ca2+, Mg2+, Fe3+, Ni2+, and Cr3+ have little influence on fluorescent enhancement.

N OOCH3

NH

NN

N

N OOCH3

HN N

N

N

+Zn2+

max= 443 nm em = 539 nm

pH 7.4

λ λ

Zn2+

Jiangli Fan, Yunkou Wu, and Xiaojun Peng



1394 A Cation-exchange Resin Promoted IminoAldol Reaction, Leading to the Synthesis of2-Isocephem and 2-Oxa-isocephem H

N

O

MeO

PMP

OMe

N

MeO

O

OSO2Me

OMeMeO

OTMS

O

OMeMeO

OMe

ONHPMP

OMe

+Amberlyst® 15 DRYO

O

PMPMakoto Shimizu, Masanori Tachi, and IwaoHachiya

1396 Preparation and Enhanced ElectrochromicProperty of Three-dimensional OrderedMesostructured Mixed Tungsten–TitaniumOxides

Minjia Yuan, Yidong Lu, Bozhi Tian, HaifengYang, Bo Tu, Jilie Kong, and Dongyuan Zhao

1398 Photochromic Properties of DiaryletheneMaleimide Derivatives in Polar Solvents

N OO

SS OMe

Me

CNN OO

SS

Me

CN

OMeR R

hν

hν'

R = HR = NO2

The compounds show photochromism in acetonitrile or in ethanol.Tadatsugu Yamaguchi and Masahiro Irie

1400 Synthesis of Dense Y-zeolite Bulks withLarge Surface Area Using a HydrothermalHot-pressing (HHP) Process

Dense Y-zeolite bulks with a higher specific surface area of approximately 800 m2/g was preparedby HHP treatment at 423 K for 2 h with 40 MPa (1.1 mm in thickness and 20 mm in diameter).

Atsushi Nakahira, Shinichi Takezoe, and YukiYamasaki

Chemistry Letters · Chemistry Letters Vol.33, No.10 (2004) C-149 Copyright 2004 The Chemical...

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Transcript of Chemistry Letters · Chemistry Letters Vol.33, No.10 (2004) C-149 Copyright 2004 The Chemical...