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Teruaki Mukaiyama, Masanori Imaoka, Toshio Izawa
1977 Volume 6 Issue 11 Pages
1257-1260
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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A new one-pot cross coupling reaction of the Grignard reagents and allyl alcohols via 2-allyloxypyridinium salt was investigated. 2-Allyloxy-1-ethyl-4,6-dimethylpyridinium salts, prepared in situ from allyl alcohols and 1-ethyl-2-fluoro-4,6-dimethylpyridinium tetrafluoroborate, reacted easily with the Grignard reagents to afford the corresponding cross coupling products in good yield.
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Katsumichi Ono, Kazuhisa Okura, Kenkichi Murakami
1977 Volume 6 Issue 11 Pages
1261-1264
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Propylene oxide was found to react easily with silica gel surfaces in the presence of water. The reaction obeyed second order kinetics with respect to the concentration of proton. Kinetic data suggested that propylene oxide was chemisorbed on the silica gel surfaces with ring opening.
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Hideki Sakurai, Mitsuo Kira, Hiroshi Umino
1977 Volume 6 Issue 11 Pages
1265-1268
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Trimethylsilylpotassium, prepared in a nonpolar solvent by the reaction of hexamethyldisilane with potassium methoxide in the presence of 18-crown-6, is a useful reagent for efficient homogeneous electron transfer. The first esr spectra of anion radicals of benzophenone and naphthalene in
n-hexane as well as those in THF and benzene were recorded.
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Kiminori Itoh, Mitsunori Sukigara, Kenichi Honda
1977 Volume 6 Issue 11 Pages
1269-1272
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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A simple method for measuring reaction rate constants of anion–cation annihilation reactions is proposed. The method is principally capable of obtaining an accurate value of the total reaction rate constant K in Eq. (4) . A preliminary result is given for the diphenylanthracene–benzonitrile system.
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Itamar Willner, Asher Gamliel, Mordecai Rabinovitz
1977 Volume 6 Issue 11 Pages
1273-1274
Published: November 05, 1977
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2,3:6,7:8,9:12,13-tetrabenzo[13]annulenyl anion
1 was prepared from the corresponding hydrocarbon
2. The effect of benzannelation and the spatial structure of the anion is derived from its proton nmr spectrum.
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Katsumi Hanji, Hazime Shimizu, Masatoshi Ono, Teiichi Homma
1977 Volume 6 Issue 11 Pages
1275-1278
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Electron microprobe Auger spectroscopy study of the surface compositional changes of a Cu-0.28 wt% Al alloy in the initial oxidation revealed that aluminum was enriched on the surface due to its selective oxidation. The degree of its enrichment was not uniform and depended on a structure of grains and on whether places were inside grains or grain boundaries.
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Yasuo Kikugawa, Masami Kawase
1977 Volume 6 Issue 11 Pages
1279-1280
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Pyridine-borane, which was readily prepared from pyridine hydrochloride and sodium borohydride, reduced oximes to the corresponding hydroxylamines in good yields with simple procedure. Other functional groups (ester, nitrile, nitro, amide, and halide) present in the same molecule of oximes were not reduced by this reagent.
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Yoshihisa Matsuda, Fukiko Kubota, Yukito Murakami
1977 Volume 6 Issue 11 Pages
1281-1284
Published: November 05, 1977
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Oxomolybdenum(V) complexes of tetraphenylporphine and octaethylporphine, Mo(O) (OC
2H
5) (TPP) and Mo(O) (OEP)X (X = Cl or OCH
3), were prepared from the corresponding porphyrins by reaction with molybdenum pentachloride. Both ESR and electronic spectra indicate that the complexes coordinated with an alkoxide group exist in dichloromethane or chloroform as a single monomeric species, while more than one species are present in aromatic solvents for each of the complexes.
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Takeshi Yamamura, Yoshio Umezawa
1977 Volume 6 Issue 11 Pages
1285-1288
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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A reversible photogalvanic effect was observed with a Pt electrode coated with an aggregate of a hydrated magnesium porphyrin. Quantum efficiencies at each wavelength were obtained from the spectral dependence of the photocurrent. A charge separation responsible for the observed photocurrent was discussed comparatively with the chlorophyll system.
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Isao Kubo, Iwao Miura, Tadao Kamikawa, Takahiko Isobe, Takashi Kubota
1977 Volume 6 Issue 11 Pages
1289-1292
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Chemical investigation of the bitter principles from
Isodon Kameba has led to the isolation and characterization of a new
ent-kaurenoid diterpene, kamebanin
1, which has in vitro cytotoxicity, in vivo tumor inhibitory, and antibacterial activities.
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Akira Sekiguchi, Wataru Ando
1977 Volume 6 Issue 11 Pages
1293-1294
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The reactions of ketones with 1-chloromethyltrimethylsilane in the presence of triphenylphosphine gave terminal olefins in good yields. The terminal olefins are formed through the Wittig type reactions of methylenetriphenylphosphorane with ketones.
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Jerald K. Rasmussen
1977 Volume 6 Issue 11 Pages
1295-1298
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Phase transfer (crown ether or quaternary ammonium salt) catalyzed reaction of benzaldoxime with potassium salts (cyanide or halide) produces a 3:1 mixture of benzonitrile and benzamide. A base-catalyzed mechanism is proposed. Extension of the procedure to provide a general, one-pot conversion of aldehydes to nitriles is indicated.
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Yuichi Yamamoto, Reiko Yoda, Kyoko Sekine
1977 Volume 6 Issue 11 Pages
1299-1300
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Thermal reaction of
N,
N-dimethyl-2,4-dithiobiuret (
1a) with monochloroacetone (
2a) in aqueous solution gave 4-methyl-2-(
N,
N-dimethylthiocarbamoyl)aminothiazole (
3a) and 5,2′-bithiazole derivative, 4-methyl-2-dimethylamino-5-(4′-methylthiazol-2′-yl)thiazole (
4a). Reaction of (
1a) and phenacyl bromide (
2b) gave 2-dimethylamino-4-phenyl-5-(4′-phenylthiazol-2′-yl)thiazole (
4b) alone in one step and in a good yield.
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Noboru Yoshida, Masatoshi Fujimoto
1977 Volume 6 Issue 11 Pages
1301-1304
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The recombination reaction of 2,4-dihydroxyazobenzene (DAB;H
*HA) with the hydroxide ion is investigated by temperature-jump method in 2% (v/v) ethanol-water solution. The presence of the minimum observed in the τ
−1 vs. \barC
OH plot is interpreted by assuming a pre-equilibrium involving an intermediate H
*A
− with an undissociated para-OH, which has not been pointed out so far.
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Seichi Okeya, Yukio Onuki, Yukio Nakamura, Shinichi Kawaguchi
1977 Volume 6 Issue 11 Pages
1305-1308
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Bis (β-diketonato)palladium(II) reacts with excess amines(L) to afford [Pd(β-dik)L
2] (β-dik) or [PdL
4] (β-dik)
2 depending upon whether L is a secondary or a primary amine, respectively. These reactions are reversible and the relative stability in solution of the complexes containing the β-diketonate anion in the outer sphere is in the order: acac < tfac < hfac.
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Hisanori Horita, Tetsuo Otsubo, Soichi Misumi
1977 Volume 6 Issue 11 Pages
1309-1312
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Three isomeric [2.2]tropyliocyclophanes were synthesized. The similarity of their structures to those of [2.2]metapara- and meta-cyclophanes and a relationship between the structures and the intramolecular CT interaction are discussed on the basis of the NMR and electronic spectra, respectively.
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Toshiyasu Ishimaru, Hitoshi Ikeda, Mariko Hatamura, Hajime Nitta, Mino ...
1977 Volume 6 Issue 11 Pages
1313-1316
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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α-Halo-β-dicarbonyl compounds are useful reagents for the protection of carboxylic acids, particularly penicillin 3-carboxylic acid. The protected carboxylic acids can be successfully converted into the free acids by treatment with nitrosating reagents such as sodium nitrite and alkyl nitrite. The probable mechanism of this deprotection is also described.
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Hitoshi Ikeda, Hajime Nitta, Mariko Hatamura, Minoru Hatanaka, Toshiya ...
1977 Volume 6 Issue 11 Pages
1317-1318
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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α-Halo-β-dicarbonyl compounds are successfully used as the carboxyl protective reagents in the synthesis of cephalexin from penicillin.
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Tran Dinh Tuong, Kenji Otsuka, Shigeo Hayano
1977 Volume 6 Issue 11 Pages
1319-1322
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The behavior of an anthraquinoid acid dye in an aqueous solution of an anionic surfactant,sodium dodecyl sulfate,was investigated by electronic spectroscopy and gel permeation chromatography. The experimental findings suggest that above the cmc, one dye molecule is associated with one surfactant micelle.
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Tran Dinh Tuong, Shigeo Hayano
1977 Volume 6 Issue 11 Pages
1323-1326
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The interaction of an anthraquinoid acid dye with a nonionic surfactant of the nonylphenol ethylene oxide type has been investigated by spectroscopic measurements and gel permeation chromatography. The results are interpreted by assuming that the dye is adsorbed on the surfactant micelles and the Freundlich isotherm has been found to correlate well the data.
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Juji Yoshimura, Ken-ichi Sato, Hironobu Hashimoto
1977 Volume 6 Issue 11 Pages
1327-1330
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Application of dimethyl sulfoxide-trifluoroacetic anhydride for the oxidation of an isolated hydroxyl group of partially protected carbohydrates gave uloses in good yields, and for that of 2,3-dihydroxyl groups of
D-glucosides followed by the reaction with carbonyl reagents gave easily 2,3-diulose derivatives.
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Takashi Handa, Sumio Goto, Toshiro Akino
1977 Volume 6 Issue 11 Pages
1331-1332
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The immobilized glucoamylase (from
Rhizopus niveus) was prepared by amidination reaction to partially imidoesterized polyacrylonitrile which had been grafted onto flaky glass surface preirradiated by electron-accelerator.
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Keitaro Hiromi, Haruko Fujimori, Junko Yamaguchi-Ito, Hiroshi Nakatani ...
1977 Volume 6 Issue 11 Pages
1333-1336
Published: November 05, 1977
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A kinetic method for the determination of ascorbic acid is described. The method is based on the linear relationship, in a wide range, between the apparent first-order rate constant,
kapp, of the reduction of 2,6-dichlorophenolindophenol by ascorbic acid and the concentration of ascorbic acid. The method is sensitive, specific, and applicable to turbid or colored samples.
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Toyoki Kunitake, Yoshio Okahata
1977 Volume 6 Issue 11 Pages
1337-1340
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Electron microscopy showed that modified dialkylammonium salts and methyldialkylsulfonium salts formed bilayers in dilute aqueous solutions. The effect of polar head groups on the aggregation properties of the amphiphiles was discussed.
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Zen-ichi Yoshida, Hisatoshi Konishi, Yasuhiro Kamitori, Hisanobu Ogosh ...
1977 Volume 6 Issue 11 Pages
1341-1344
Published: November 05, 1977
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Cationic diaminocyclopropenylidene mercury complexes (
1) were synthesized by the reaction of diaminocyclopropenium perchlorate with mercury acetate. Coordination of two diaminocyclopropenylidenes to divalent mercury was confirmed on the basis of microanalyses and spectral measurements. The value of
13C–
199Hg coupling constant in
1 indicates a diagnostic of sp hybridization of the C–Hg bond.
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Yoshiaki Echigo, Yutaka Watanabe, Teruaki Mukaiyama
1977 Volume 6 Issue 11 Pages
1345-1346
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Treatment of methyl thiocarbamates with 2-chloro-3-ethylbenzoxazolium tetrafluoroborate and triethylamine at room temperature affords isocyanates in good yields under neutral condition.
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Teruo Shinmyozu, Takahiko Inazu, Tamotsu Yoshino
1977 Volume 6 Issue 11 Pages
1347-1350
Published: November 05, 1977
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[3.3]Paracyclophane-5,8-quinone I was synthesized. Its charge-transfer absorption maximum at 406 nm (ε 407) showed a marked red shift as compared with that of [2.2]- and [4.4]paracyclophanequinones.
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Takashi Joh, Nobue Hagihara
1977 Volume 6 Issue 11 Pages
1351-1354
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The influence of pressure on the insertion reactions of alkynes into
trans-chlorohydrido-bis(triethylphosphine)platinum(II) was investigated under high pressures up to 10,000 kg/cm
2. It was found that the insertion reactions of alkynes into H–Pt(II) bond were generally accelerated with increasing pressure and the influence of pressure was remarkable in the reactions which proceeded via an ionic intermediate. In some cases change of reaction mechanisms by the pressure changes was observed.
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Masakazu Yamashita, Kiyoshi Mizushima, Yoshihisa Watanabe, Take-aki Mi ...
1977 Volume 6 Issue 11 Pages
1355-1358
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Carboxylic esters were prepared under mild conditions in high yields from alkyl halides and alkoxides using pentacarbonyliron as a carbonylating reagent.
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Naomichi Furukawa, Fujio Takahashi, Toshiaki Yoshimura, Shigeru Oae
1977 Volume 6 Issue 11 Pages
1359-1360
Published: November 05, 1977
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Dimethyl sulfoximine was tested as a solvent in the S
N2 reactions and was shown to have characteristic features of both protic and polar aprotic solvents. Dimethyl sulfoximine, when used as a mixed solvent with methanol, showed a large rate acceleration of the S
N2 reaction likely DMSO or DMF.
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Yusuke Ujihira, Yoshinori Kobayashi, Tsutomu Nomizu
1977 Volume 6 Issue 11 Pages
1361-1364
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Positron lifetime measurements in aqueous solutions of pyridine-hydrochloric acid at various solute concentrations revealed that pyridinium ion, formed by Py + H
+\
ightleftharpoons [PyH]
+ reduced the relative intensity of ortho-positronium(I
2) without changing ortho-positronium lifetime(τ
2) significantly. Comparison of the result with that of anilinium ion suggested that the presence of pyridine ring, whose π electron density is lower than that of benzene, is an important point for the reduction of I
2.
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Tohru Sakakibara, Akinori Seta, Yoshifusa Tachimori, Tetsuyoshi Takamo ...
1977 Volume 6 Issue 11 Pages
1365-1366
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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The Michael reaction of the 3-nitro-2-enopyranoside
1 with ethyl malonate in THF or with acetone in the presence of small amounts of NaOH gave the mannopyranoside
2 or
3, respectively, whereas the similar reaction with acetylacetone afforded a mixture of the mannopyranoside
4 and the altropyranoside
5.
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Masahiko Tsuchiya
1977 Volume 6 Issue 11 Pages
1367-1370
Published: November 05, 1977
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Precursors of ions with excess kinetic energy (KE ions) have higher internal energy than those of ordinary ions (thermal ions), so that rearrangement reactions like H/D scrambling may be less probable in the mass spectra of KE ions. For example, the location and number of deuterium atoms in 1,4-butanediol-2,2,3,3-d
4 has been correctly indicated by the mass spectrum of KE ions, while the ordinary mass spectrum gives no reliable information because of rearrangement. Information obtained from mass spectrum of KE ions has also been described.
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Tatsuro Ouchi, Takeshi Yamada, Minoru Imoto
1977 Volume 6 Issue 11 Pages
1371-1374
Published: November 05, 1977
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It was found that an aqueous solution of sodium chondroitin sulphate (ChS-Na) can initiate a radical polymerization of methyl methacrylate (MMA) in the presence of Cu(II)-ion. The kinetic behavior with respect to ChS-Na and MMA was studied. The initiation mechanism was considered to be as follow: ChS-Na forms a hydrophobic area in water. MMA is incorporated into the area, where the complex of ChS/Cu(II)-ion/MMA/H
2O generates free radicals of MMA, which initiate the polymerization.
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Yasuhiko Yoshida, Shohei Inoue
1977 Volume 6 Issue 11 Pages
1375-1376
Published: November 05, 1977
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1-Ethoxyethyl carbamate was obtained directly by the reaction of ethyl vinyl ether with carbon dioxide and amine such as dimethylamine and diethylamine.
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Nobuyuki Yamamoto, Hiroyoshi Kanai, Kimio Tarama
1977 Volume 6 Issue 11 Pages
1377-1378
Published: November 05, 1977
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1,3-Butadiene was selectively hydrogenated to
cis-2-butene by cobalt(I)-bipyridyl complexes. The order of the addition of butadiene to cobalt complexes determined the distribution of products. The catalytic activity was affected by the bipyridyl/cobalt ratio and halide anions.
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Kiyoshi Tanaka, Takeshi Nakai, Nobuo Ishikawa
1977 Volume 6 Issue 11 Pages
1379-1382
Published: November 05, 1977
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The title reagent
3, readily generated in situ from the reaction of 2,2,2-trifluoroethoxybenzene (
1) with lithium diisopropylamide, was found to be useful for the preparation of 2-phenoxy-2-alkenoic acids (
6) from various carbonyl compounds via facile acid hydrolysis of the initially formed difluorovinylcarbinols (
5).
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Kiyoshi Isobe, Yukio Nakamura, Shinichi Kawaguchi
1977 Volume 6 Issue 11 Pages
1383-1386
Published: November 05, 1977
Released on J-STAGE: March 27, 2006
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Oxidative substitution of tetrakis(triphenylphosphine) nickel(0) with a chloro- or bromo-pyridine takes place in toluene at room temperature to afford a dimeric complex, [NiX(σ-pyridyl) (PPh
3)]
2. The σ-pyridyl nickel(II) complex is very stable and has a strong preference for the dimeric structure, the bridging ligand being readily replaced by other halide and pseudo halide ions. [NiCl (2σ-C
5H
4N) (PPh
3)]
2 acts as a very powerful catalyst for completely selective cross coupling between 2-chloropyridine and methylmagnesium bromide.
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Gohei Yoshida, Hideo Kurosawa, Rokuro Okawara
1977 Volume 6 Issue 11 Pages
1387-1388
Published: November 05, 1977
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Insertion of RC≡CR (R= COOCH
3) or 2,5-norbornadiene into the Pd–C bond of Pd(Ph
3P) (CH
2SCH
3) (OCOCF
3) gave the corresponding
cis-addition product in good yield. Pd(Ph
3P) (CH
2SCH
3)Cl was unreactive toward RC≡CR (R= COOCH
3), however, the reaction between these two compounds occurred readily by addition of catalytic amount of AgClO
4 to give [Pd(CR=CRCH
2SCH
3)Cl]
2 (R= COOCH
3).
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