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Joung Hee Lee, Akira Matsumoto, Masayuki Yoshida, Osamu Simamura
1974 Volume 3 Issue 9 Pages
951-954
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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Heating aromatic or heteroaromatic compounds carrying a carbonyl and an arylazo group at adjacent nuclear positions with triethyl phosphite resulted in the formation of a 1,2-diazole ring through reductive cyclizations. Similar, but oxidative, cyclizations were effected by the action of selenium dioxide on compounds with a methylene group at an appropriate position.
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Motoyasu Saito, Tadayoshi Morita, Kahei Takase
1974 Volume 3 Issue 9 Pages
955-958
Published: September 05, 1974
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3
H-Cyclohept[
a]azulen-3-one (azuleno[1,2-
d]tropone) (
1) was synthesized, starting from 2-styrylazulene (
2). In trifluoroacetic or dil. sulfuric acid,
1 exists in hydroxycyclohept[
a]azulenylium ion (A
1), while it exists in a dication (C) in cone. sulfuric acid.
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Masaaki Iwata, Sakae Emoto
1974 Volume 3 Issue 9 Pages
959-960
Published: September 05, 1974
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The aldol condensation of several aromatic aldehydes with acetone was specifically catalyzed by cupric ion and the additional effect of zinc ion on the cupric-ion catalyzed condensation was substantiated.
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Akio Kato, Yoko Suyama
1974 Volume 3 Issue 9 Pages
961-962
Published: September 05, 1974
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Titanium dioxide powders of 98 % rutile content were obtained by vapor phase reaction of TiCl
4–H
2–CO
2 system at temperatures above 1000 °C. The average particle sizes of products were 0.11∼0.66 μ. The sizes decreased with increasing reaction temperatures.
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Masayuki Kitadani, Chizuko Kabuto, Kunikazu Sakai, Akira Yoshikoshi, Y ...
1974 Volume 3 Issue 9 Pages
963-966
Published: September 05, 1974
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Upon heating in formic acid dolabradiene (1) gives a mixture of hydrocarbons. Five backbone rearrangement products isolated from the mixture are assigned to Δ
5(10)-8β-rimuene (2), Δ
5(10)-rimuene (3), Δ
1(10)-rimuene (4), Δ
8(9)-pimaradiene (5), and Δ
1(10),5-rimutriene (6a), respectively. Their formation mechanisms are also discussed.
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Shigeru Kobayashi
1974 Volume 3 Issue 9 Pages
967-970
Published: September 05, 1974
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Synthesis of new pyrimidine-fused 1,4-benzodiazepines
(3 and
4) was achieved by heating the corresponding 1,4-benzodiazepines (
1) with formamide in the presence of phosphoryl chloride.
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Takayuki Suga, Toshifumi Hirata, Nobuo Iwata
1974 Volume 3 Issue 9 Pages
971-974
Published: September 05, 1974
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The structure of alnuserrudiolone, a new C
31-dammarane-type triterpene isolated from the male flowers of
Alnus serrulatoides Call. (Betulaceae), has been elucidated to be (20
s)-12β,20-dihydroxy-24-methylene-dammaran-3-one (I) by a combination of chemical and spectroscopic methods.
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Eiichi Arai, Makoto Takahasi
1974 Volume 3 Issue 9 Pages
975-978
Published: September 05, 1974
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Ion impact reaction of methanol was studied with accelerated inert gas ions with initial energy from 2–6 kV. It is shown that the yields are linear vs. lnE
i, and the ratio of the average logarithmic energy loss to the reaction probability (α⁄p
j) was determined. The dependence of α on mass of the projectile ion is discussed.
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Sumio Ichiba, Motomi Katada, Hisao Negita
1974 Volume 3 Issue 9 Pages
979-982
Published: September 05, 1974
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Tin sesquisulfide, Sn
2S
3, was obtained as a single phase through thermal decomposition of SnS
2. The Mössbauer parameters of the phase were not the same as those of the mixture of SnS and SnS
2 and were consistent with those of Sn
2S
3.
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Nobufumi Maki
1974 Volume 3 Issue 9 Pages
983-986
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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The
cis-[Cr
III(CN)
2en
2]ClO
4 complex gave rise to a two-stepped wave responsible for the reductions of Cr(III) to Cr(II) and to Cr(I) state at the dropping mercury electrode(DME) in dimethyl sulfoxide(DMSO). The reduction of the first step is reversible, while that of the second is quasi-reversible. The standard redox potential of the Cr(III)/Cr(II) couple was −1.586 V (vs. aq. SCE). In aqueous solutions containing 0.5 M Na
2SO
4 or acetate buffer, however, the
cis-[Cr(CN)
2en
2]
+ ion gave rise to only one irreversible wave for the reduction of Cr(III) to Cr(II) even in the presence of ethylenediamine in a large excess. Unlike the cases of
cis-[Co(CN)
2en
2]
+ and
cis-[Co(CN)
2dip
2]
+, the aquation of the resulting Cr(II) complex occurs so fast that a cyanide disproportionate reaction cannot be observed under such conditions.
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Hisashi Okawa, Mitsunori Tanaka, Sigeo Kida
1974 Volume 3 Issue 9 Pages
987-988
Published: September 05, 1974
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The novel binuclear hetero-metal complex, CuNi(fsacen)·3H
2O, was synthesized, where H
4fsacen denotes
N,
N′-ethylenebis(3-carboxysalicylaldimine). This complex has [CuN
2O
2]- and [NiO
6]-chromophores and two metal ions are connected by the phenolic oxygens. The magnetic susceptibility was well explained in terms of the equation for the high-spin nickel(II)-copper(II) cluster.
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Tomitsugu Taketatsu, Noriko Kono
1974 Volume 3 Issue 9 Pages
989-992
Published: September 05, 1974
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In absorption spectra of heavier rare earth (Gd to Lu) chelates of Chlorophosphonazo III, the absorption bands extend from 700 to 800 nm with a maximum at approximately 745 nm. The intensity of these bands increases with an increase in the mole ratio of the metal to the reagent and in the atomic number. Also it depends upon the pH value and the elapsing time. The corresponding chelates of lighter rare earths (La to Eu) do not exhibit a similar maximum under the same conditions.
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Norio Koine, Hiroyuki Yamaguchi, Teiichi Tanigaki, Jinsai Hidaka, Yoic ...
1974 Volume 3 Issue 9 Pages
993-996
Published: September 05, 1974
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Potassium
trans(
N)-(
C-methyl substituted ammoniatriacetato)(β-alaninato)cobaltate(III) have been prepared, where
C-methyl substituted ammoniatriacetates are (
S)-alaninate-
N,
N-diacetate and (
R,
S)- or (
S,
S)-alaninate-
N-isopropionate-
N-acetate. Some of the possible isomers concerning the arrangement of three feet of the tripod-like quadridentate ligand have been isolated and assigned structurally on the basis of the nuclear magnetic resonance spectra and isomerization experiments.
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Keiji Iriyama, Masahiko Yoshiura, Hiroshi Asai
1974 Volume 3 Issue 9 Pages
997-1000
Published: September 05, 1974
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Chlorophyll b (Chl-b) in methanol solution absorbing at 650 nm (Cb65O) forms microcrystals absorbing at 680 nm after the addition of water. In methanol-dioxane-water solutions. Chl-b molecules form an aggregate absorbing at 672 nm (Cb672). Cb672 was obtained either by mixing a small volume of a methanol-dioxane solution of Chl-b with a large volume of water, or by mixing a large volume of methanol-water solution of the pigment with a small volume of dioxane.
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Takashi Matsumoto, Sachihiko Imai, Hideto Masuda, Kenji Fukui
1974 Volume 3 Issue 9 Pages
1001-1004
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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In order to examine the fragmentation reaction of tricyclic diterpenoids, 6α-hydroxy-7-oxoabieta-8,11,13-triene (V) was prepared from 7-oxoabieta-8,11,13-triene (XI) via an enol acetate (XII). After V was treated with
p-toluenesulfonyl chloride, the product was heated at 200°C to afford a β-naphthol derivative (IX).
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Jasjit S. Walia, Sudhir N. Bannore, Amrik S. Walia, Larry Guillot
1974 Volume 3 Issue 9 Pages
1005-1008
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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The reaction of benzaldehyde, 2-aminobenzenecarbothioamide, potassium cyanide, and acetic acid yields tetrahydroquinazolinethione
7 and/or α-aminonitrile
11 under different conditions. These results are used to support the intermediacy of an imine
3 or its immonium ion in the formation of α-aminonitriles
5.
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Yasuhiko Shirota, Takashi Nogami, Yoshiki Hasegawa, Hiroshi Mikawa
1974 Volume 3 Issue 9 Pages
1009-1012
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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A new mechanism has been proposed for the tricyanovinylation reaction of aromatic amines with tetracyanoethylene.
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Teruaki Mukaiyama, Takeshi Takeda, Kunio Atsumi
1974 Volume 3 Issue 9 Pages
1013-1014
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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In the presence of AlCl
3, trimethylsilyl sulfides react with α,β-unsaturated acetals to give γ-alkoxyallyl sulfides in good yields.
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Morio Yagihara, Yoshio Kitahara, Toyonobu Asao
1974 Volume 3 Issue 9 Pages
1015-1019
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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Photolytic decomposition of 2-diazophenol in methanol afforded 6-hydroxy-6-methoxy-2-(2-hydroxyphenylazo)fulvene, guaiol, phenol, and dimer of methyl cyclopentadienecarboxylate. The decomposition in water gave 6,6-dihydroxyfulvene derivative. Thermal decomposition of 2-diazophenol gave fulvenylidenebenzo-1,3-dioxole. Structure and mechanism of the formation of these products are discussed.
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Toru Taguchi, Yuzuru Takahashi, Mitsuomi Itoh, Akira Suzuki
1974 Volume 3 Issue 9 Pages
1021-1024
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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Trialkylboranes are readily electrolyzed by using graphite as an anode in a sodium perchlorate-methanol solution containing sodium methoxide or a sodium acetate-acetic acid solution to give corresponding alkyl methyl ethers or alkyl acetates in good yields, respectively.
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A. C. Jain, R. K. Gupta
1974 Volume 3 Issue 9 Pages
1025-1028
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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Kaempferol (
1) when reacted with 2-hydroxy-2-methyl-3-butene in the presence of borontrifluoride etherate yielded a mixture of 6,8-di-(3-methylbut-2-enyl) derivative (
2), 4″, 5″-dihydro-6″, 6″-dimethyl pyrano (2″,3″ : 7,8)-kaempferol (
3) and 8-(3-methylbut-2-enyl) derivative (
4). The orientation of alkenyl unit in compound 4 has been unambiguously established and then it agrees in direct comparison with natural noranhydroicaritin.
1Complete acetylation of 4, followed by reaction of 5 with one mole of methyl iodide in the presence of dry K
2CO
3 and acetone afforded 8-(3-methylbut-2-enyl)-rhamnocitrin triacetate (
6) which on deacetylation finally gave natural isoanhydroicaritin
1(
7).
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Shonosuke Zen, Eisuke Kaji, Haruo Kohno
1974 Volume 3 Issue 9 Pages
1029-1030
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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Anomeric mixture (α:β = 4:3 by NMR integration) of 4-nitro-2,3,4,6-tetradeoxyhexopyranose (
1) could be synthesized from acrolein and 1-nitro-2-propanol in a reasonable yield. When α- and β-anomer of 2 were hydrogenated in the presence of Raney Nickel, the respective methyl
DL-tolyposaminides were obtained; α- and β-anomer of
N-benzoyl derivatives (
4) of
3 were identical with the authentic samples.
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Jun Yamauchi
1974 Volume 3 Issue 9 Pages
1031-1034
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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The paramagnetic resonance of polycrystalline 1,3-bisdiphenylene-2-(
p-chlorophenyl)-allyl can be observed in the temperature region above 3.25 K. Below the temperature the anomalous resonance absorptions, which may be the antiferromagnetic resonance, were observed. This may be the first experimental observation in organic free radicals.
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Takehiko Ito, Yasuo Takami
1974 Volume 3 Issue 9 Pages
1035-1036
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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Active methylene compounds such as cyclohexanone and acetophenone are carboxylated by the reaction with carbon dioxide in the presence of ferric ethoxide under mild conditions to give β-ketoacids.
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Kunio Okamoto, Tomomi Kinoshita
1974 Volume 3 Issue 9 Pages
1037-1040
Published: September 05, 1974
Released on J-STAGE: March 27, 2006
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The existence of a linear free-energy relationship between the phenolic reactivity and the selectivity for attack of the phenol molecule on carbonium ion intermediates has been established for the titled substrates. The examples are the first ones for the reaction between the carbonium ions and an ambident molecule.
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Kazuhisa Hiratani, Takeshi Nakai, Makoto Okawara
1974 Volume 3 Issue 9 Pages
1041-1044
Published: September 05, 1974
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Bromination of the title compounds
1 resulted in the formation of the corresponding 2-dimethylamino-4-bromomethyl-1,3-dithiolan-2-ylium bromide (
2) via regiospecific (S-5) participation by the dithiocarbamate function, irrespective of substitution on the γ-carbon atom. This is in contrast to the
C-protonation of
1 in which the ratio of S-5 vs. S-6 depends on the γ-substitution.
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Tsutomu Nagasao, Haruka Yamada
1974 Volume 3 Issue 9 Pages
1045-1050
Published: September 05, 1974
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The Raman spectra of pyridine, triethylamine, dimethylsulfoxide and maleic anhydride adsorbed on porous Vycor glass were measured and compared with results on other silicas. The spectral changes upon adsorption are interpreted to be due to the hydrogen bond formation with the surface OH groups.
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Koji Yamamoto, Masao Nakazaki
1974 Volume 3 Issue 9 Pages
1051-1054
Published: September 05, 1974
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Starting from (+)-[8]paracyclophane-10-carboxylic acid optically active [8][8]paracyclophane was prepared and its absolute configuration was correlated to (
S)-(+)-[2.2]paracyclophane-4-carboxylic acid. The absolute configurations of (−)-[8][10]paracyclophane and related optically active paracyclophanes were also discussed.
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Toshihiro Yamase, Hiroh Hayashi, Tsuneo Ikawa
1974 Volume 3 Issue 9 Pages
1055-1056
Published: September 05, 1974
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Iso-propylammonium dimolybdate dihydrate, which shows a photochromic activity in the solid state and forms a blue color in the aqueous solution on exposure to UV, has been investigated by ESR. It was confirmed that the signal responsible for the color corresponded to the formation of Mo(V).
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Toyoki Kunitake, Yoshio Okahata
1974 Volume 3 Issue 9 Pages
1057-1060
Published: September 05, 1974
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The hydrolysis of
p-nitrophenyl acetate by a polymer catalyst containing the hydroxamate and imidazole functions includes the formation of acetyl hydroxamate and its subsequent decomposition assisted by the intramolecular imidazole group. The overall catalytic efficiency is enhanced by the presence of these complementary nucleophilic functions.
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Sumio Ichiba, Motomi Katada, Hisao Negita
1974 Volume 3 Issue 9 Pages
1061-1064
Published: September 05, 1974
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The thermal decomposition products of SnSe
2 and SnSSe were investigated by Mössbauer effect. No intermediate decomposition product was found. Tin(IV) selenosulfide decomposes to tin(II) selenosulfide, which is an isomorphous compound of SnS and SnSe.
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Hiroshi Yoshida, Hironori Matsuura, Tsuyoshi Ogata, Saburo Inokawa
1974 Volume 3 Issue 9 Pages
1065-1068
Published: September 05, 1974
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NMR spectra of alkoxythiocarbonylmethylenetriphenylphosphoranes (II; R=Me, Et, i-Pr) show existence of cis and trans isomers. Alkylation of II took place exclusively at sulfur in quantitative yields. The effects of solvents and alkylating reagents on the products ratio (III
cis/III
trans)were also studied.
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Iwao Ojima, Shin-ichi Inaba, Yoichiro Nagai
1974 Volume 3 Issue 9 Pages
1069-1072
Published: September 05, 1974
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It was found that silyl enol ethers reacted with
p-toluenesulfonyl isocyanate to afford either
N-sulfonyl-2-silyloxycycloalkanecarboxamides or
N-sulfonyl-4-silyloxy-2-azetidinones. Both adducts were easily hydrolyzed to the corresponding
N-sulfonyl-2-oxoalkanecarboxamides.
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Mikio Hori, Tadashi Kataoka, Hiroshi Shimizu
1974 Volume 3 Issue 9 Pages
1073-1076
Published: September 05, 1974
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It was proved that the reaction between 9-phenylthioxanthene 10-oxide (II) and organometallic reagents proceeds through the formation of 9-phenylthioxanthenyl radical. A new method of synthesis of thiaänthracene derivative was found by the reaction of II with aryllithium.
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Teruaki Mukaiyama, Hiroshi Ishikawa
1974 Volume 3 Issue 9 Pages
1077-1078
Published: September 05, 1974
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In the presence of TiCl
4, α,β-unsaturated acetals react with Gringard reagents to give the corresponding allyl ethers in good yields.
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Hiromu Hayashi, Kengo Kawasaki, Tsutomu Murata
1974 Volume 3 Issue 9 Pages
1079-1080
Published: September 05, 1974
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A new catalyst, NH
4Cl–CuCl, for the synthesis of benzophenone azine is proposed. The recovery of expensive CuCl should be simplified than in the case of ZnCl
2–CuCl. An improved catalyst, NH
4Cl–CuCl·Ph
2C=NH, is also descrived.
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Yoshiya Harada, Koichi Ohno, Kazuhiko Seki, Hiroo Inokuchi
1974 Volume 3 Issue 9 Pages
1081-1086
Published: September 05, 1974
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To study the interaction between the Walsh orbitals of cyclopropane rings and its adjacent π-orbitals the photoelectron spectrum of dispiro[2.2.2.2]deca-4,9-diene has been measured by using the 21.22 eV helium resonance line. The first four bands in the PE spectrum have been assigned on the basis of a modified CNDO/2 approximation.
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Katsuhiko Miyoshi, Koro Sakata, Hayami Yoneda
1974 Volume 3 Issue 9 Pages
1087-1088
Published: September 05, 1974
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The addition of tetraalkylammonium bromides R
4NBr(R = C
2H
5,
n-C
3H
7 and n-C
4H
9) did not enhance Pfeiffer effect of [Zn(phen)
3]
2+-
l-strychnine system in water, while (CH
3)
4NBr enhanced it like simple salts. This could be best interpreted by assuming that hydrophobic R
4N
+ ions interfere with hydrophobic interaction between [Zn(phen)
3]
2+ and strychnine cation (stryH
+), by forming hydrophobic bonding with [Zn(phen)
3]
2+ and/or stryH
+.
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Hiroshi Kato, Kei Yamaguchi, Hiroshi Tezuka
1974 Volume 3 Issue 9 Pages
1089-1090
Published: September 05, 1974
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Photolysis of 2,3-diphenylnaphthoquinone oxide resulted in carbon–carbon bond cleavage to give a seven-membered mesoionic benz[
d]oxepine-1,5-dione intermediate, which was trapped by
N-phenylmaleimide and norbornadiene.
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Takeshi Takemura, Hiroaki Baba, Yoshio Shindo
1974 Volume 3 Issue 9 Pages
1091-1096
Published: September 05, 1974
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The phosphorescence spectrum of naphthalene has been measured in fluid isooctane solution in the temperature range of 80 to −100°C. The spectrum is essentially different from that obtained in rigid solution at 77K, and is ascribable to phosphorescence from the triplet excimer of naphthalene. An analysis of the experimental results suggests that the radiative rate constant for the triplet decay is enhanced as a result of the formation of the triplet excimer.
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Keishi Kato, Takashi Nogami, Masaaki Yokoyama, Hiroshi Mikawa
1974 Volume 3 Issue 9 Pages
1097-1100
Published: September 05, 1974
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The intrinsic photoconductivity of
N-ethylcarbazole single crystal induced by a Q-switched ruby laser was investigated. The experimental results show that charge carriers are uniformly generated in the bulk of the crystal by the photoionization of excitons produced by two-photon absorption.
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Mikio Hori, Tadashi Kataoka, Hiroshi Shimizu, Ken’ichi Narita, S ...
1974 Volume 3 Issue 9 Pages
1101-1106
Published: September 05, 1974
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Synthesis and structure of novel ylidic thiabenzenes, 1-cyano-and benzoyl-2-methyl-2-thianaphthalenes (VI and X), are discussed. The reactions of VI with several electrophiles such as dimethyl acetylenedicarboxylate, methyl propiolate, diphenylcyclopropenethione, and diphenylcyclopropene are described together with the mechanisms of the reactions.
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Kazuhiko Morio, Satoru Masamune
1974 Volume 3 Issue 9 Pages
1107-1111
Published: September 05, 1974
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The lowest energy minimum is calculated for two systems, bicyclo[3.1.0]hex-3-yl and tricyclo[3.1.1.0
2’
4]hept-6-yl, and corresponds to the C
3v and C
2v structures, respectively.
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Seiji Shinkai, Toyoki Kunitake
1974 Volume 3 Issue 9 Pages
1113-1116
Published: September 05, 1974
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Thiamine (Vitamin B
1) and its analogue, 3-methylbenzothiazolium iodide serve as suitable imine substrates for reduction by 1-benzyl-1,4-dihydropyridine, and the reduction of the imino group to amine occurs easily at room temperature.
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