-
Akinori Hasegawa, Takatoshi Yamaguchi, Michiro Hayashi
1980 Volume 9 Issue 6 Pages
611-612
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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ESR spectra of (CH
3)
xSnH
4−x− (x=0∼3) radical anions formed in TMS matrices were observed. These radical anions have trigonal bipyramidal structure and the methyl groups prefer the equatorial positions to the axial positions of the trigonal bipyramid.
View full abstract
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Kazuo Mukai, Nobuhito Iida, Yoshiko Kumamoto, Hiroyuki Kohama, Kazuhik ...
1980 Volume 9 Issue 6 Pages
613-616
Published: June 05, 1980
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A galvinoxyl derivative of benzo-15-crown-5 (
1) has been synthesized, and the complex formation between the spin labeled crown ether (
1) and the alkali metal thiocyanate has been studied by ESR measurement. A typical triplet ESR spectrum was observed for the potassium complex in ethanol rigid matrix at 77 K, clearly indicating the (1:2) complex formation between the KNCS salt and the
1. On the other hand, the sodium complex showed a symmetrical single line, suggesting the (1:1) complex formation between the NaNCS salt and the
1.
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Sigeru Torii, Hirosi Okumoto, Hideo Tanaka
1980 Volume 9 Issue 6 Pages
617-618
Published: June 05, 1980
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An efficient preparation of α,α-dimethoxyalkanoates (
2) has been performed by electrolytic desulfurization of α-(2-benzothiazolylthio) alkanoates (
1) in MeOH containing CuCl
2 as a catalytic additive, yielding
2 (94–57%) together with disulfide
3 (88–48%).
View full abstract
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Seizo Tamagaki, Kazuhiko Hotta, Seizi Kozuka
1980 Volume 9 Issue 6 Pages
619-620
Published: June 05, 1980
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The oxidation of 1,2-dithiole-3-thiones with MCPBA or NaIO
4 gives the sulfines in good yield, while the reactions with O
21, O
3, NaOCl, and BPO produce 1,2-dithiole-3-ones which are formed via the sulfines as transient intermediates.
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Yoshiro Yamashita, Mituo Masumura
1980 Volume 9 Issue 6 Pages
621-622
Published: June 05, 1980
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The photochemical reaction of tricyclic
N-iminopyridinium ylides afforded 1
H-1,2-diazepines containing novel structures by the selective electrocyclic ring closure followed by ring opening.
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Katsumi Tanaka, Koshiro Miyahara, Ken-ichi Tanaka
1980 Volume 9 Issue 6 Pages
623-626
Published: June 05, 1980
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Co-isomerization of d
0- and d
8-
cis-2-butene was carried out on a novel catalyst, MoO
x/β-TiO
2(2.9>x>2.3), which is active for olefin metathesis reaction without inter- and intra-molecular hydrogen scrambling of olefins. The ratio, d
4/(d
0+d
8), in produced
trans-2-butene was found to be zero at the initial stage of the reaction, indicating a type of cis–trans isomerization by intra-molecular metathesis.
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Kazuo Yamashita, Keiko Miyoshi, Atsuhiro Osuka, Hitomi Suzuki
1980 Volume 9 Issue 6 Pages
627-628
Published: June 05, 1980
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The photocurrent quantum yields of para-substituted tetraphenylporphyrins were found to be increased by electron-donating groups. Semi-logarithmic plots of the quantum yields vs. the half-wave potentials for the first ring oxidations of the porphyrins or the Hammett σ of substituents yielded a linear relationship.
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Akira Hanaki
1980 Volume 9 Issue 6 Pages
629-630
Published: June 05, 1980
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Cu(II)-glycylglycine chelates with cysteine forming red-purple transient. A transient which is formed immediately upon mixing the reactants is a ternary Cu(II) complex. Another transient is a binary Cu(II) complex of cysteine produced successively from the ternary complex. Spectrophotometric properties of those transients are discussed.
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Yutaka Fujise, Katsuyuki Mlwa, Shô Itô
1980 Volume 9 Issue 6 Pages
631-632
Published: June 05, 1980
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Stereoisomeric tyriverdins A and B were isolated from
Thais clavigera. The former, which is identical with tyriverdin isolated by Baker, was confirmed by
13C-NMR spectrum to be 2,2′-bis(methylthio)-6,6′-dibromo-2,2′-diindoxyl . None of these compounds are detected in the gastropod, suggesting that they are formed during the isolation process probably from tyrindoxyl sulfate, a genuine constituent.
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Hitomi Suzuki, Ichiro Hidaka, Atsuhiro Osuka, Akemi Iwasa, Tadashi Mis ...
1980 Volume 9 Issue 6 Pages
633-634
Published: June 05, 1980
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Nitration of 2,5-dimethylthiophene with copper(II) nitrate in acetic anhydride gives 2,5-dimethyl-3-nitrothiophene and 3,2′-methylene (2,5-dimethylthiophene) (5′-methylthiophene) as major products. Treatment of 3,4-dibromo-2,5-dimethylthiophene with nitric acid (d = 1.5) in dichloromethane in the presence of a catalytic amount of sulfuric acid yields 3,4-dibromo-5-methyl-2-nitrooxymethylthiophene as the sole major product.
View full abstract
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Teruaki Mukaiyama, Katsumi Fujimoto, Takuji Hirose, Takeshi Takeda
1980 Volume 9 Issue 6 Pages
635-638
Published: June 05, 1980
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Highly optically pure β-substituted γ-butyrolactones (V) were obtained in good yields by the reaction of (
E)-(2
R,3
S)-6-alkylidene-3,4-dimethyl-2-phenylperhydro-1,4-oxazepine-5,7-dione (I) with phenylthiomethyllithium, followed by i) treatment with trimethyloxonium tetrafluoroborate and ii) acid hydrolysis.
View full abstract
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Sigeru Torii, Tsutomu Inokuchi, Nobu Hasegawa
1980 Volume 9 Issue 6 Pages
639-640
Published: June 05, 1980
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A new procedure for arylselenenylation of enones has been developed by electrolysis with diaryl diselenide and chlorotrimethylsilane in methanol. In the course of the reaction generation of aryl selenols in situ is assumed.
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Tetsuo Suami, Yutaka Honda
1980 Volume 9 Issue 6 Pages
641-644
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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Aminocyclitol antibiotic fortimicin B has been synthesized by condensation of 2,6-bis-
N-(2,4-dinitrophenyl)-α-6-
epi-purpurosaminyl chloride and 1,2:4,5-di-
N,
O-carbonylfortamine B, followed by removal of all protective groups.
View full abstract
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asanobu Hidai, Tamotsu Takahashi, Ichiro Yokotake, Yasuzo Uchida
1980 Volume 9 Issue 6 Pages
645-646
Published: June 05, 1980
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Treatment of
cis-[W(N
2)
2(PMe
2Ph)
4] with 2-propanol/KOH yields hydrazine, whereas use of n-alcohols instead of 2-propanol gives ammonia as a main nitrogen hydride. Metal hydrides such as [(η
5-C
5H
5)
2ZrHCl], [H
2Fe(CO)
4] and [NaAlH
2(OCH
2CH
2OCH
3)
2] also react with the above dinitrogen complex to give ammonia in moderate yield.
View full abstract
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Katumitu Hayakawa, Kazuto Ohara, Iwao Satake
1980 Volume 9 Issue 6 Pages
647-650
Published: June 05, 1980
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The circular dichroism spectrum of poly(
L-lysine)(PLL) in aqueous 1-octanesulfonate solution was measured as a function of surfactant concentration at varying temperatures and the conformational phase diagram was constructed. At temperatures above 10°C, the increase in surfactant concentration causes PLL to change stepwise from coil to β-form and from β-form to helical conformation, Upon lowering temperature, the surfactant concentration range, where PLL assumes β-form, becomes narrower and eventually disappears at around 10°C.
View full abstract
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Sei-ichi Hayashi, Takeshi Nakai, Nobuo Ishikawa
1980 Volume 9 Issue 6 Pages
651-654
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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Defluorinative hydrolysis (or alcoholysis) of
gem-difluoroolefins (
1) easily prepared via the facile difluoromethylenation of carbonyl compounds afforded the carboxylic acids (or esters). The homologation method was applied to the synthesis of anti-inflammatory
ibuprofen. Furthermore, defluorinative hydrolysis of monofluoroolefins obtained via the reduction of
1 gave the aldehydes.
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Shigeru Futamura, Hiroyuki Ohta, Yoshio Kamiya
1980 Volume 9 Issue 6 Pages
655-658
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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Irradiations of 6-cyanophenanthridine in the presence of electron-rich olefins afforded the corresponding azocine and azetidine derivatives regiospecifically via their exciplex intermediates.
View full abstract
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Egle M. Beccalli, Luisella Majori, Alessandro Marchesini, Clara Torric ...
1980 Volume 9 Issue 6 Pages
659-662
Published: June 05, 1980
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Irradiation of (3, 5)[9]isoxazolophanes (I) afforded the corresponding azabicyclo [1O.1.O]tridec-13(1)-en-11-ones (II) from which the [9]oxazolo- (III) and the [9]imidazolo-phanes (V) were obtained.
View full abstract
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Hiroshi Miyamae, Yoshinaho Numahata, Miharu Nagata
1980 Volume 9 Issue 6 Pages
663-664
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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The crystal structure of the title compound has been determined by X-ray diffractometry. Two dimethylsulphoxide molecules co-ordinate to the Pb atom through their O atoms in trans position. The skeletal structure is a linear chain of [>Pb⟨
II⟩] unit.
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Mitsuko Onoda, Masanobu Saeki
1980 Volume 9 Issue 6 Pages
665-666
Published: June 05, 1980
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A new type of Ti
2S
3 was prepared by reducing TiS
2 in an H
2S–H
2atmosphere at 600°C. The structure is proposed to be of 6R-type, being composed of cubic-close-packed sulfur layers as well as the fully and partially occupied titanium layers. The ordering of titanium vacancies was suggested.
View full abstract
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Hiroshi Nishihara, Takehiko Mori, Taro Saito, Yukiyoshi Sasaki
1980 Volume 9 Issue 6 Pages
667-668
Published: June 05, 1980
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Formation of ammonia and hydrazine was quantitatively analyzed in the reaction of
cis-W(N
2)
2(PMe
2Ph)
4 with acidic hydridometal carbonyls, H
2Fe(CO)
4 or HFeCo
3(CO)
12 after treatment of the products with aqueous KOH.
View full abstract
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Hidetaka Yatagai, Yoshinori Yamamoto, Kazuhiro Maruyama
1980 Volume 9 Issue 6 Pages
669-670
Published: June 05, 1980
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Regioselective coupling between lithium acetylides and allylic halides is realized by using lithium iodide as an additive.
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Toshifumi Kageyama, Tamotsu Yamamoto
1980 Volume 9 Issue 6 Pages
671-672
Published: June 05, 1980
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Electrolytic oxidation of tetraalkylammonium bromides to give the corresponding bromites was found. This method is convenient and applicable to the preparation of the stable tetraalkylammonium bromites.
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Yukimichi Nakao, Shoei Fujishige
1980 Volume 9 Issue 6 Pages
673-676
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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Addition of sodium hydroxide to colloidal nickel boride in ethanol resulted in a marked enhancement of its catalytic activity for atmospheric hydrogenation of acetone at 30°C by a factor of more than 20. Other ketones and aldehydes with bulky substituents were smoothly hydrogenated by the activated colloidal catalyst.
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Hirokazu Maeda, Yoshiyuki Hayashi, Kazuhiro Teramura
1980 Volume 9 Issue 6 Pages
677-678
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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Cross-linked polystyrene supported tertiary amines and amine oxides are found to be a very efficient catalyst for a nucleophilic substitution reaction. The amine oxide resin (MPE-5-AO) was one of the most effective and economical catalysts and can be used several times without the loss of the catalytic activity.
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Tsuneo Sato, Makoto Watanabe, Ryoji Noyori
1980 Volume 9 Issue 6 Pages
679-682
Published: June 05, 1980
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The first, stereocontrolled entry to 1′, 4′-dialkylated pyrimidine
C-nucleosides is outlined.
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Hiroyasu Inoue, Tsunehisa Mori, Tadamitsu Sakurai
1980 Volume 9 Issue 6 Pages
683-686
Published: June 05, 1980
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Benzil shows dual phosphorescence in an ethylene glycol glass at 77 K. The short-lived phosphorescence at 504 nm is assigned to near-planar transoid geometry. Evidence indicates that the long-lived one appearing three maxima at 402 nm, 427 nm, and 460 nm is due to medium imposed near-planar cisoid geometry.
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Shin Sato, Takashi Kitamura, Shigeru Tsunashima
1980 Volume 9 Issue 6 Pages
687-690
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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The formation of α- and β-alanine in the photolysis of hydrogen azide in propionic acid was confirmed by the NMR spectra. The yield ratios, alanine/nitrogen and β/α in alanine were found to be 0.4 and 1.5, respectively, suggesting that NH(
1Δ) radicals insert into the C–H bonds of propionic acid.
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Yasuo Sakai, Yoshito Tobe, Yoshinobu Odaira
1980 Volume 9 Issue 6 Pages
691-692
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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The synthesis of bicyclo[
n, 2.2]bridgehead alkenes (
2a) and (
2b) by the solvolytic rearrangement of the corresponding tricyclic acetates (
3a) and (
3b) in acetic acid and the electrophilic addition of acetic acid to
anti-Bredt olefin (
2a) are described.
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Masayasu Iida, Hideo Yamatera
1980 Volume 9 Issue 6 Pages
693-694
Published: June 05, 1980
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The Hg
2+-assisted aquation of
cis-[CoCl(OH
2)(phen)
2]
2+ was retarded by sodium methanesulfonate and benzenesulfonate(0.5–1.0 mol dm
−3), while they accelerated a similar reaction of [CoCl(NH
3)
5]
2+.The unusual retardation effect has been attributed to the hydrophobic interaction of the complex ion and the organic sulfonate ions.
View full abstract
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Sigeru Torii, Noboru Sayo, Hideo Tanaka
1980 Volume 9 Issue 6 Pages
695-698
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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Regioselective attack of the trivalent phosphorus atom of dialkyl and trialkyl phosphites on either nitrogen or sulfur atom of sulfenamides has been found. The reaction of phenylsulfenamides with dialkyl phosphites yielded phosphorothiolates, whereas the treatment of (2-benzothiazolyl)sulfenamides with dialkyl and trialkyl phosphites gave phosphoramidates in excellent yields.
View full abstract
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Yoshiko Shiki, Fujiko Yamaoka, Michiro Hayashi
1980 Volume 9 Issue 6 Pages
699-702
Published: June 05, 1980
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Microwave spectra of ethyl fluoride and its deuterated species were measured in the ground, methyl torsional and skeletal bending excited states. Fermi resonance between the second excited methyl torsional state and the first excited skeletal bending state was analyzed in relation to the methyl internal rotation.
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Michio Kondo, Kouji Okamoto, Ichiro Nishi, Makoto Yamamoto, Tetsuo Kat ...
1980 Volume 9 Issue 6 Pages
703-704
Published: June 05, 1980
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Replacement reaction of peptide NH with chlorine was applied to the peptide antibiotics, gramicidin S and tuberactinamine N. The rate of chlorination followed by NMR spectra demonstrates that the hydrogen-bonded peptide NH in the molecule is much more susceptible to chlorination than the solvent-exposed peptide NH.
View full abstract
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Hiroshi Irie, Hiromi Nakanishi, Nobutaka Fujii, Yukio Mizuno, Tamaki F ...
1980 Volume 9 Issue 6 Pages
705-708
Published: June 05, 1980
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N-Methoxycarbonyl (MOC)-amino acids regenerate the parent amino acids by treatment with dimethyl sulphide and methanesulphonic acid. Synthesis of MSH-Release Inhibiting Factor was accomplished using MOC-amino acids and applying the above mentioned deblocking method.
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Toshio Goto, Makoto Onaka, Teruaki Mukaiyama
1980 Volume 9 Issue 6 Pages
709-712
Published: June 05, 1980
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S-(2-Pyridyl) thioates, especially derived from secondary and tertiary carboxylic acids, are decarbonylated by use of a catalytic amount of nickel chloride and zinc powder to give olefins in good yields.
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Seiichiro Ogawa, Tatsushi Toyokuni, Tetsuo Suami
1980 Volume 9 Issue 6 Pages
713-716
Published: June 05, 1980
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Penta-
N,
O-acetyl-
DL-valienamine, and its related branched-chain unsaturated aminocyclitols and cyclitols were synthesized from the dibromides derived from tri-
O-acetyl-
DL-(1,3/2)-4-methylene-5-cyclohexene-1,2,3-triol.
View full abstract
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Hiroshi Kato, Kazue Tani, Haruki Eurumisawa, Yoshiko Tamura
1980 Volume 9 Issue 6 Pages
717-720
Published: June 05, 1980
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Photooxidation of several mesoionic compounds gave ring cleavage products, some of which were apparently formed via the endoperoxides of the mesoionic rings. Photooxidation of a Δ
2-oxazolin-4-one and a Δ
2-thiazolin-4-one gave the corresponding 4,4′-bisoxa- and bisthiazolinone in dichloromethane, whereas the former gave benzamide in dimethylformamide.
View full abstract
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Hideyuki Matsumoto, Kazuhiro Ohkawa, Taichi Nakano, Yoichiro Nagai
1980 Volume 9 Issue 6 Pages
721-724
Published: June 05, 1980
Released on J-STAGE: March 27, 2006
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In the presence of a catalytic amount of triphenylphosphine, 1,1,2,2-tetrachloro-1,2-dimethyldisilane reacted smoothly under mild conditions with carbon tetrachloride to produce (trichloromethyl) methyldichlorosilane
1 in good yield. (Trichloromethyl)dimethylchlorosilane was also readily prepared by the triphenylphosphine-promoted transfer of the trichloromethyl group from
1 to dimethyldichlorosilane.
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Krystian Kloc, Jacek Mlochowski, Ludwik Syper
1980 Volume 9 Issue 6 Pages
725-728
Published: June 05, 1980
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Benzo- and naphthoquinones bearing oxiranyl or 1,3-dioxolan-2-yl substituents were prepared by oxidative demethylation of appropriate hydroquinone dimethyl ethers with silver (II) dipicolinate. A remarkable selectivity of this silver (II) complex as an oxidizing reagent was demonstrated.
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Sotaro Miyano, Masayoshi Nawa, Harukichi Hashimoto
1980 Volume 9 Issue 6 Pages
729-730
Published: June 05, 1980
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From easily resolved 2,2′-diamino-1,1′-binaphthyl were prepared axially dissymmetric bisphosphine ligands, (
R)- and (
S)-2,2′-bis(diphenylphosphinamino)-1,1′-binaphthyl; the rhodium-catalyzed asymmetric hydrogenation of α-acylaminoacrylic acids and esters gave the corresponding amino acids of up to 95% optical purity.
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Koichi Mizuno, Toru Kamuki, Masaomi Suzuki
1980 Volume 9 Issue 6 Pages
731-734
Published: June 05, 1980
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Large amounts of hydrogen cyanide (HCN), acetonitrile, acrylonitrile, and propionitrile were formed in the reduction of NO with propylene and H
2–CO over Al
2O
3 supported Pt and Rh catalysts. Rh was more active in both the reduction of NO and the formation of HCN and nitriles than Pt. Propylene employed as a reducing agent was more reactive in the conversion of NO into HCN than H
2–CO.
View full abstract
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Hamao Watanabe, Tsutomu Muraoka, Yasuhiro Kohara, Yoichiro Nagai
1980 Volume 9 Issue 6 Pages
735-736
Published: June 05, 1980
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Peralkylcyclopentasilanes [R
2Si]
5 (where R=Et, Pr, Bu and
i-Bu) were prepared by the reactions of corresponding dialkyldichlorosilanes (R
2SiCl
2) with lithium.
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Takeji Chikamoto, Shogo Nagata
1980 Volume 9 Issue 6 Pages
737-738
Published: June 05, 1980
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An improved gas chromatographic method is presented for the determination of trace amount of nitrite ion (NO
2−) in water. The method is based on the Sandmeyer reaction, i.e., the diazotization of
p-bromoaniline by NO
2− followed by reaction with CuCl in hydrochloric acid to form
p-bromochlorobenzene. The derivative is determined by gas chromatography, employing an electron capture detector. The detection limit for NO
2− is 0.5 ng/ml (ppb).
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Tsuguo Tanaka
1980 Volume 9 Issue 6 Pages
739-742
Published: June 05, 1980
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Rearrangement of 2,2′-spirobichroman derivatives having electron donating substituents into 4,4′-dihydroxy-1,1′-spirobiindane analogues was effected by boiling solution of the former in HBr- or HI-HBr-acetic acid.
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Masaru Matsuoka, Yoshinobu Makino, Toshio Takei, Teijiro Kitao
1980 Volume 9 Issue 6 Pages
743-744
Published: June 05, 1980
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The reaction of 1,4-dihydroxyanthraquinone with ethylenediamine in the presence of Cu(I)Cl or Cu(II)Cl
2 gave 6-hydroxy-1,2,3,4-tetrahydronaphtho- (2, 3-f) -quinoxaline- 7,12-dione in quantitative yield at ambient temperature. The reaction was promoted greatly by copper ions. The possible mechanism and the role of copper ions were discussed.
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Yoshiyuki Kiso, Takeshi Hirokawa
1980 Volume 9 Issue 6 Pages
745-748
Published: June 05, 1980
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A method for the isotachophoretic determination of stability constant was examined by a computor analysis of the observed isotachopherograms. The obtained values for acetate complexes with Ba, Ca, Zn, Cd, Cu and Ca-tartrate complex were compared with those obtained by the other methods and discussed. The present method is applicable even for mixed samples.
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Yumihiko Yano, Yutaka Hoshino, Waichiro Tagaki
1980 Volume 9 Issue 6 Pages
749-752
Published: June 05, 1980
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The reactions of aldehydes with thiazolium ions and flavin were investigated in the presence of CTABr micelle. The reactions were found to be facilitated by a cationic micelle.
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Masanobu Hidai, Masami Orisaku, Yasuzo Uchida
1980 Volume 9 Issue 6 Pages
753-754
Published: June 05, 1980
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Cyclopropane was carbonylated by [Rh(CO)
2Cl]
2 under carbon monoxide pressure to give cyclobutanone, dipropyl ketone, propyl isopropyl ketone, and 2- or 3-methylcyclohexanone. Some other cyclopropane derivatives were also examined. Norcarane gave a small amount of bicyclo[4.2.0]octa-7-one, though phenylcyclopropane did not give any carbonylation products. The formation of polyketone was efficient in the case of methylenecyclopropane.
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Daisuke Uemura, Chuji Katayama, Akio Wada, Yoshimasa Hirata
1980 Volume 9 Issue 6 Pages
755-756
Published: June 05, 1980
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Crystal and molecular structure of palythene isolated from
Palythoa tuberculosa (Coelenterata) was unambiguously determined by X-ray analysis including its absolute configuration. The structure of palythene was defined as an inner salt and then features of delocalization of the positive charge were elucidated.
View full abstract
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Tetsuya Kato, Hisao Kondo, Yukishige Kitano, Go Hata, Yoshikazu Takagi
1980 Volume 9 Issue 6 Pages
757-760
Published: June 05, 1980
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(±)-3,6-Epoxy-5-hydroxy-5,6-dihydro-3-ionol was synthesized from β-ionone via 3,6-dihydroxy-α-ionone and its structure including the relative configurations was established as (±)-2β,5β-epoxy-2α-[3α-hydroxy-1(
E)-butenyl]-1β,3,3-trimethylcyclohexan-1α-ol by X-ray analysis.
View full abstract
