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Yukihiko Naka, Yukio Yamamoto
1992 Volume 21 Issue 12 Pages
2263-2264
Published: 1992
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Preparation of fine particles of poly(
N,
N′-methylenebisacrylamide) by radiation-induced polymerization is described. The size of the obtained fine particles is 0.22 μm having a narrow distribution. This result is one of the examples of the particle formation promoted by the crosslinking polymerization. This is the first report on poly(
N,
N′-methylenebisacrylamide) fine particles.
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Katsuo Shinozaki, Kazuhiro Mizuno, Hirohisa Oda, Yukio Masaki
1992 Volume 21 Issue 12 Pages
2265-2268
Published: 1992
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The C(6)-carbon degradation and elimination of C(4)-hydroxy group of D-glucosamine were achieved in 8-steps and 30% overall yield to furnish (4
R, 5
S)-5-vinyl-2-oxazolidinone-4-carbaldehyde dimethyl acetal, which was utilized as a key intermediate for enantiospecific synthesis of biologically important threo β-hydroxy-γ-amino acids, natural (3
S, 4
S)-statine and (3
S, 4
S)-AHPPA
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Masashi Ishikawa, Yoshiharu Matsuda, Kazuhiko Yamamoto, Shunichi Fukuz ...
1992 Volume 21 Issue 12 Pages
2269-2272
Published: 1992
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The acid-catalyzed reactions of 1,5-dihydroriboflavin-2′,3′,4′,5′-tetraacetate (FlH
2) with quinones (Q) result in the one-electron oxidation of FlH
2 to FlH
2+• and the two-electron reduction of Q to the hydroquinones (QH
2) in the presence of HClO
4 in acetonitrile. In the presence of Me
4NOH, the base-catalyzed reactions result in the two-electron oxidation of FlH
2 to Fl and the one-electron reduction of Q to Q
−•.
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Shinji Yamada, Masakatsu Matsumoto
1992 Volume 21 Issue 12 Pages
2273-2276
Published: 1992
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Irradiation of levoglucosenone having a 6-membered cyclic α,β-unsaturated ketone structure with a high pressure mercury arc stereoselectively produced (
Z)-β,γ-unsaturated acid derivatives. The mechanism of the formation of these products is explained in terms of the α-cleavage reaction which is scarcely observed in the photochemical reaction of α,β-unsaturated ketones.
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Yoshiki Hirata, Kouki Nukanobu, Masayuki Hara, Yasuo Asada, Jun Miyake ...
1992 Volume 21 Issue 12 Pages
2277-2280
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In order to build up stable Langmuir-Blodgett (LB) film of the photosynthetic reaction centers (RC) from
Rhodopseudomonas viridis, effect of the formation of polyion complex between charged residues of RC and water soluble polyions was examined. Cationic polymer, poly-L-lysine (PLL), enhanced the stability of RC LB films during the film preparing process whereas anionic polymer, poly-L-glutamate, induced complete denaturation of RCs. LB films of RCs prepared with PLL show reproducible surface pressure area isotherm and high transfer ratio of RC monolayer to solid substrate.
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Kunio Mochida, Shigeru Masuda, Yoshiya Harada
1992 Volume 21 Issue 12 Pages
2281-2284
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Photoelectron spectra of permethylated linear germanes display isolated bands in the 7.70–8.60 eV region, which are readily assigned to ionizations from the germanium framework.
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Atsushi Ishihara, Masatoshi Nomura, Toshiaki Kabe
1992 Volume 21 Issue 12 Pages
2285-2288
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Catalyst derived from alumina-supported ruthenium carbonyl-alkali metal hydroxide systems remarkably increased the catalytic activity in hydrodesulfurization of dibenzothiophene compared with an alumina-supported ruthenium carbonyl, ruthenium acetylacetonate or ruthenium chloride system to give biphenyl selectively.
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Akihiko Ishii, Meng-Xin Ding, Juzo Nakayama, Masamatsu Hoshino
1992 Volume 21 Issue 12 Pages
2289-2292
Published: 1992
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The reaction of the dihydrazone of 2,2,6,6-tetramethyl-1,7-diphenyl-1,7-dione with Se
2Cl
2 in refluxing benzene in the presence of tributylamine gave the corresponding 1-oxo-7-selone and 1,7-diselone derivatives in 14 and 33% yields, respectively, while similar reaction of the dihydrazone of 2,2,5,5-tetramethyl-1,6-diphenyl-1,6-dione gave bicyclic 1,3-diselenetane (25%), 1,2,4-triselenolane (20%), and cyclohexene (12%) derivatives by intramolecular cyclizations.
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Takashi Tominami, Kiyonori Ikeda, Tatsuya Nabeshima, Yumihiko Yano
1992 Volume 21 Issue 12 Pages
2293-2296
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It was found that N(3)-H dissociation of 10-methylisoalloxazine plays a crucial role for a rate-accelerating metal ion effect on the oxidation of N-benzyl-1,4-dihydronicotinamide (BNAH) in MeCN.
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Tatsumi Ishihara, Yuichiro Nishi, Kazuhiro Kometani, Yukako Mizuhara, ...
1992 Volume 21 Issue 12 Pages
2297-2300
Published: 1992
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Effects of additives on CO
2 sensing characteristics were studied on CuO–BaTiO
3 mixed oxide capacitor. Although the operating temperature shifted slightly to a higher temperature and the response time was prolonged, sensitivity to CO
2 was increased by the addition of ZnO, Bi
2O
3, SrO, and Ag. In particular, CuO–BaTiO
3 mixed oxide added with Ag was highly sensitive and selective for CO
2 detection.
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Masaharu Komiyama, Manabu Kirino
1992 Volume 21 Issue 12 Pages
2301-2302
Published: 1992
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Scanning tunneling microscopy (STM) images of silicon oxide surface and of Pt ultrafine particles deposited on it were obtained for the first time. The silicon oxide sample employed consists of a thin (ca. 0.7 nm thick) native silica film present on a Si(100) surface. The STM observation of these sample systems was critically dependent on the choice of the electron tunneling conditions.
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Takuzo Funabiki, Koji Kashiba, Takehiro Toyoda, Satohiro Yoshida
1992 Volume 21 Issue 12 Pages
2303-2306
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Linear and branched alkanes are monooxygenated with O
2 in nonheme iron complex/hydroquinone systems. Selectivity to form either alcohols or carbonyl compounds was controlled by the pyridine concentration. Reactivity of different types of C-H bonds was affected by the substituents of hydroquinones, suggesting that hydroquinones are located in the vicinity of an active center in the product formation step.
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Hiroshi Tsukube, Jun’ichi Uenishi, Hiromi Higaki, Ken’ichi ...
1992 Volume 21 Issue 12 Pages
2307-2310
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Lanthanide complex with bipyridine-armed crown ether was first demonstrated to mediate effective transport of hydrophilic HisOMe and LysOEt salts via two-point binding.
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Masaru Mizoguchi, Philip F. Low
1992 Volume 21 Issue 12 Pages
2311-2314
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Infrared spectra of 0.12 mm thick frozen NaCl solution from 1600 to 4000 cm
−1 were obtained at sub-zero temperature with a FTIR spectrometer. The transmittance of the sample decreased sensitively with decreasing temperature around the frequency of 2700 cm
−1. The volume fraction of ice in the NaCl solution, calculated from the absorbance at 2700 cm
−1, agreed well with the values predicted from a phase diagram of the system H
2O-NaCl.
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Yoshiko Urabe, Kanichiro Takamizawa
1992 Volume 21 Issue 12 Pages
2315-2318
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DSC curves for henpentacontane and dopentacontane, when crystallized from the melt, showed anomalous sharp endothermic peaks on the region of the high-temperature phases. Grounding the samples made the peaks disappear. The appearance of the peak may be ascribed to the kinetic factors, not to the first order phase transition.
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Isamu Shiina, Teruaki Mukaiyama
1992 Volume 21 Issue 12 Pages
2319-2320
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Various carboxylic esters are prepared in good to excellent yields by the reaction of equimolar amounts of silyl derivatives of carboxylic acids and alcohols by using a catalytic amount of active Lewis acid in hexamethyldisiloxane, a solvent.
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Yohji Misaki, Hiroyuki Nishikawa, Kazuya Kawakami, Shiro Koyanagi, Tok ...
1992 Volume 21 Issue 12 Pages
2321-2324
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Synthesis of the title compound (
1), and its molecular structure determined by X-ray crystallographic analysis, and electrochemical property investigated by cyclic voltammetry are described. Several cation radical salts of
1 have been prepared by electrochemical oxidation method, and their electrical properties are also presented.
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Yuzo Nishida, Miyuki Nasu, Tetsuya Akamatsu, Miyuki Tanno
1992 Volume 21 Issue 12 Pages
2325-2328
Published: 1992
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We have observed that the binuclear manganese(III/IV) compounds with di-μ-oxo bridge exhibit solvent-dependent solution ESR spectra at room temperature, and have concluded that there are two ESR-detectable species, electron-localized and electron-delocalized ones, in the solution.
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Kunio Hiroi, Yoshihisa Arinaga, Takashi Ogino
1992 Volume 21 Issue 12 Pages
2329-2332
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A dramatic solvent effect was observed on the nickel-catalyzed asymmetric rearrangement of a cyclopropane system into an optically active cyclopentane derivative with chiral phosphine ligands. The stereochemistry of the product was readily controlled by selecting the catalyst, nickel or palladium, with extremely high enantioselectivity.
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Minoru Tsuda, Takayuki Ishida, Takashi Nogami, Sadamu Kurono, Mamoru O ...
1992 Volume 21 Issue 12 Pages
2333-2334
Published: 1992
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Benzyne generated by the reaction of 2-aminobenzoic acid and pentyl nitrite in a refluxing benzene was found to add to C
60 in good yield. The reaction products were separated by HPLC to give C
60(C
6H
4), C
60(C
6H
4)
2, C
60(C
6H
4)
3, and C
60(C
6H
4)
4, which were confirmed by mass spectra.
1H NMR spectrum of C
60(C
6H
4) is consistent with the structure of mono-addition product, whereas those of C
60(C
6H
4)
2, C
60(C
6H
4)
3, and C
60(C
6H
4)
4 indicate that they consist of the corresponding mixtures of isomers.
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Takashi Matsuno, Masumi Koishi
1992 Volume 21 Issue 12 Pages
2335-2338
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Hydroxyapatite powders having various average particle diameters were prepared by a wet process and by the calcination under various conditions. Porous sintered bodies of hydroxyapatite having relative densities of 49.4–85.8% were obtained by heating green compact bodies. The fracture toughness of these sintered bodies was measured by a Single-Edge V-Notched Beam(SEVNB) method. The fracture toughness increased linearly with an increase in relative density.
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Yutaka Nishigaichi, Manabu Fujimoto, Kihei Nakayama, Akio Takuwa, Kens ...
1992 Volume 21 Issue 12 Pages
2339-2342
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By the TiCl
4-coordination to the ethereal functionality on the pentadienyltin, its addition to aldehydes was controlled to proceed at its γ-position with high regioselectivity, in contrast to the usual ε-selectivity of dienyltins and -silanes. High
syn,syn-stereoselectivity was simultaneously realized as an asymmetric induction from the tin reagent.
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Toshifumi Hirukawa, Minoru Oguchi, Norinobu Yoshikawa, Tadahiro Kato
1992 Volume 21 Issue 12 Pages
2343-2344
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A spirocyclic lactone, curcumanolide A, was synthesized from homogeranyl cyanide in 11 steps in racemic form by using Br
+-induced cyclization and subsequent ring contraction method.
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Isao Yagi, Shoji Kaneko
1992 Volume 21 Issue 12 Pages
2345-2348
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SnO
2 thin films have successfully been grown from di-n-butyltin diacetate on a heated glass substrate by a pneumatic spraying system. The effects of film growth parameters,
i.e., film thickness, film growth rate, and substrate temperature on the microstructures of the films were studied by X-ray diffraction and scanning electron microscopy. The SnO
2 films of preferably oriented (200) plane were grown under the optimum growth conditions.
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Masatoshi Abe, Kozo Toyota, Masaaki Yoshifuji
1992 Volume 21 Issue 12 Pages
2349-2352
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Novel 1-amino-2-aryldiphosphenes carrying 2,6-bis(trifluoromethyl)phenyl or 2,4,6-tris(trifluoromethyl)phenyl group as an aryl substituent were prepared and the push-pull substituent effect on –P=P– was demonstrated by
31P NMR.
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Yutaka Ukaji, Katsuhiko Inomata
1992 Volume 21 Issue 12 Pages
2353-2356
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One carbon homologation reaction of γ-silicon substituted allylic alcohols was found to proceed by the treatment with triethylaluminium followed by diethylaluminium chloride and diiodomethane to afford homoallylic iodides instead of the corresponding cyclopropanes. Silicon function introduced to γ-position was crucial for the homologation reaction.
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Ermitas Alcalde, Maria Gisbert, Lluïsa Pérez-Garcia
1992 Volume 21 Issue 12 Pages
2357-2360
Published: 1992
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The first synthesis of the hitherto unknown ethyleneimidazolium benzimidazolate inner salts is described. Their dipolar structure is well reflected on the basis of the
1H and
13C NMR parameters. Under neutral and mild conditions the title compounds underwent a type of β-elimination, affording their corresponding 2-vinyl-1
H-benzimidazoles in high yields.
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Yuko Hirose, Hiroshi Yamaoka, Haruo Akashi, Hiroshi Nozaki, Tomoyuki F ...
1992 Volume 21 Issue 12 Pages
2361-2362
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From (+)-catechin under radical reaction with 2,2′-azobis(2-methylpropionitrile), a novel intramolecular cyclization product was isolated and its structure has been characterized to be 2,4′,5′,12-tetrahydroxy-9,10-benzo-7-oxatricyclo[6.2.2.0
1,6]dodeca-2,5,9-trien-4-one by the spectroscopic analyses and the chemical transformation.
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Taku Matsuo, Hiroshi Nakamura, Takuya Nakao, Mitsuhiro Kawazu
1992 Volume 21 Issue 12 Pages
2363-2366
Published: 1992
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Second-harmonic-generation (SHG) was clearly observed with ultrathin poly(vinyl chloride) films (ca. 25 nm), impregnated with amphiphilic ruthenium tris(2,2′-bipyridine) complexes. On the basis of SHG intensity from multi-layered assembly of the thin film, the laser-induced polarization of the second harmonic wave was concluded to have a big component in perpendicular direction with respect to the film surface.
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Ei-ichi Negishi, Thinh Nguyen, John P. Maye, Daniele Choueiri, Noriyuk ...
1992 Volume 21 Issue 12 Pages
2367-2370
Published: 1992
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Competitive β-hydrogen abstraction of “mixed” dialkylzirconocenes and kinetic measurements of decomposition of methyl(alkyl)zirconocenes reveal unexpected relative reactivity of alkyl groups as β-hydrogen donors, such as
s-Bu >
t-Bu ≥ Et >
n-Bu >
i-Bu, which correlate well in most cases with the reactivity order of: β-methyl > β-methylene > β-methine. Some mechanistically crucial features of the reaction are also discussed.
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Tsunenori Nozawa, Mitsushi Nishimura, Masahiro Hatano
1992 Volume 21 Issue 12 Pages
2371-2374
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High resolution
13C NMR spectra in solid states were observed for chlorophyll a and pheophorbide a with a high magnetic field spectrometer. The rate constants of cross polarization (
TCH) and
1H spin-lattice relaxation time in the rotating frame (
T1ρH) were determined. The rate constants and relaxation times reflected structural differences among them.
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Naomi Sakai, Chieko Fukui, Yoshikazu Shizuri
1992 Volume 21 Issue 12 Pages
2375-2378
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Cyclamenoside, a glucoside ester of gallic acid was isolated from
Cyclamen persicum Miller as a potent inhibitor of hydrogen peroxide release from peritoneal neutrophils of rat. The structure of the active compound was determined by some chemical reactions and mainly by using
1H and
13C NMR spectroscopy.
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Yoshitaka Nagao, Shigeyoshi Katagiri
1992 Volume 21 Issue 12 Pages
2379-2380
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35Cl NQR spectra of N-Cl bonds were measured for CCl
3CONHCl, CHCl
2CONHCl, CH
2BrCONHCl and Cl(CH
2)
2CONHCl. The ionic character of N-Cl bonds was estimated for these compounds according to Townes and Dailey. The ionic character was compared with the yield of the 1,2-addition to cyclohexene under the photochemical reaction. The yield increased as the value of the ionic character neared zero.
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Akihiko Kudo, Tadayoshi Sakata
1992 Volume 21 Issue 12 Pages
2381-2384
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Decomposition of N
2O into N
2 and O
2 at room temperature was demonstrated on a Pt/TiO
2 photocatalyst in the presence of water vapor. The photocatalytic activity was enhanced by the participation of photocatalytic decomposition of water.
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Tushar K Chakraborty, Azhar K Hussain, Subodh P Joshi
1992 Volume 21 Issue 12 Pages
2385-2388
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An efficient convergent route to the first total synthesis of 9(R)-N-BOC-Ahda methyl ester, in optically pure form, is described.
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Masaki Kawano, Takehide Watanabe, Kazuko Matsumoto
1992 Volume 21 Issue 12 Pages
2389-2392
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Mono- and binuclear ruthenium compounds with mercapto ligands were stepwise synthesized from hydrogen sulfide and [Ru(II)H(S
2CNMe
2) (CO) (PPh
3)
2]. The molecular structures were determined by X-ray crystallography. These compounds are unstable to air.
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Yoshikazu Sugihara, Jun-ichi Kanemaru, Junji Saito, Ichiro Murata
1992 Volume 21 Issue 12 Pages
2393-2396
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An oxidation product of 3-bromo-1-formyl-4-[(2,4,6-cycloheptatrienyl)(phenylthio)methyl]azulene with
m-chloroperbenzoic acid was transformed into 3-bromo-1-formyl-4-(E)-styrylazulene upon standing at 0 °C in a solid state. A similar rearrangement was also observed in the oxidation of 3-chloro-1-methyl-[(2,4,6-cycloheptatrienyl)(phenylthio)methyl]azulene.
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Kiyoshi Otsuka, Masaharu Hatano
1992 Volume 21 Issue 12 Pages
2397-2400
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Alkaline earth element-added boron and phosphorus mixed oxides supported on Cab-O-Sil showed high catalytic activity in partial oxidation of methane to HCHO at < 773 K. The results of the experiment using
18O
2 suggested that the lattice oxygen atoms of the catalyst are responsible for the oxidation.
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Hiroshi Uyama, Yasuhiro Matsumoto, Shiro Kobayashi
1992 Volume 21 Issue 12 Pages
2401-2404
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Emulsion copolymerization of styrene with a block-type amphiphilic poly(2-oxazoline) macromonomer having a polymerizable styryl group was performed. The macromonomer possessing the polymerizable group attached to the hydrophobic segment gave monodisperse polymer particles. On the other hand, the macromonomer having polymerizable group linked to the hydrophilic segment produced particles with broad size distribution.
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Toshio Fuchigami, Shinji Ichikawa, Akinori Konno
1992 Volume 21 Issue 12 Pages
2405-2408
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N-(2,2,2-Trifluoroethylidene)sulfenamides (trifluoromethylated sulfenimines) were easily prepared in one step by anodic oxidation of 2,2,2-trifluoroethylamine and diaryl disulfides in MeCN/Et
4NClO
4 using MgBr
2 as a redox mediator. The sulfenimines were highly useful building blocks for the preparation of trifluoromethylated amines, aminoketone, and aminoalkanoates.
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Kunio Hiroi, Mitsuhiro Haraguchi, Yoko Masuda, Jun Abe
1992 Volume 21 Issue 12 Pages
2409-2412
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The palladium-catalyzed allylations of chiral hydrazones bearing phosphine groups were executed successfully under neutral reaction conditions with various allylating reagents, affording optically active α-allyl carbonyl compounds. The systematic and stereochemical investigation of these reactions shows that the intramolecularly-substituted phosphine groups served as chiral ligands and the anionic counterparts in the allylating reagents were markedly stereoelectronically effective on asymmetric induction.
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Tsuneji Sano, Hiroshi Yanagishita, Yoshimichi Kiyozumi, Dai Kitamoto, ...
1992 Volume 21 Issue 12 Pages
2413-2414
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Separation of ethanol/water mixture was carried out by pervaporation through a silicalite membrane on a porous stainless steel support. It was found that the membrane has the high ethanol permselectivity with a separation factor α(EtOH/H
2O) of approximately 60.
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Nagao Kobayashi, Shin-ichiro Nakajima, Tetsuo Osa
1992 Volume 21 Issue 12 Pages
2415-2418
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Several tetraazaporphyrins (TAPs) have been characterized by electronic absorption, fluorescence, and magnetic circular dichroism (MCD) spectroscopy, together with electrochemical methods. The absorption coefficients (ε) and band positions change markedly with changing TAP structure and solvent. The potential differences of the redox couples of tetra-
tert-butylated TAP skeleton are closer to those in general porphyrins than phthalocyanines (Pcs).
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Shu Kobayashi, Shun-ya Onozawa, Teruaki Mukaiyama
1992 Volume 21 Issue 12 Pages
2419-2422
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6-Deoxy-D-allose is prepared from simple achiral starting materials, butynal and chloroacetic acid, via two key steps of the chiral tin(II) triflate mediated asymmetric aldol reaction and the dihydroxylation using osmium tetroxide.
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Mikio Nakamura
1992 Volume 21 Issue 12 Pages
2423-2426
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Low spin ferric porphyrin complexes carrying rapidly rotating 1-methylimidazole and rotationally fixed 2-isopropylimidazole have been prepared. Chemical shift range of the pyrrole protons at −56 °C was nearly twice as much as that of the bis(hindered imidazole) complex. Orientation of the fixed ligand relative to the porphyrin plane was determined based on the splitting pattern of the
meso-
13C signals.
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Jianzhuang Jiang, Ken-ichi Machida, Eiji Yamamoto, Gin-ya Adachi
1992 Volume 21 Issue 12 Pages
2427-2430
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The electronic behaviors of sandwich-type rare earth octaethylporphyrinates Ln(oep)
2 and Ln
2(oep)
3 (Ln = Ce, Pr, and Eu) were characterized by measurements of the near infrared or UV-vis spectra and D.C. conductivity. However, no remarkable change induced by oxidation of the ligand from (oep)
2− to (oep·)
− was observed on the conductivity.
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Noriyuki Akane, Yoshinori Kanagawa, Yutaka Nishiyama, Yasutaka Ishii
1992 Volume 21 Issue 12 Pages
2431-2434
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Samarium(II) iodide equivalent was generated from metallic samarium and Me
3SiCl/Nal reagent in acetonitrile under ambient conditions. Dehalogenation of α-halocarbonyl compounds and reductive coupling of ketones were successfully carried out by the use of the samarium(II) species, thus generated, in acetonitrile.
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Masaaki Mishima, Kazuhide Nakata, Hideyuki Nomura, Mizue Fujio, Yuho T ...
1992 Volume 21 Issue 12 Pages
2435-2438
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Gas phase basicities of α-t-butylstyrenes were determined based on the proton transfer equilibria. The substituent effect on the basicity has been analyzed by means of the LArSR Eq. 1, providing a ρ of −12.5 and an r of 0.86. The reduced r value relative to that for α-methylstyrene may be attributed to sterically twisting out of the coplanarity of benzene π-system in the conjugate acid ion, α-t-butyl-α-methylbenzyl cation.
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Masaaki Mishima, Chul Hyun Kang, Mizue Fujio, Yuho Tsuno
1992 Volume 21 Issue 12 Pages
2439-2442
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Gas phase basicities of styrenes toward Me
3Si
+ have been determined based on Me
3Si
+ transfer equilibria. The substituent effect on the stability of Me
3Si-styrene
+ complex has been analyzed by means of the LArSR Eq., giving a ρ value of −5.76 and an r value of 0.41. These results imply that Me
3Si-styrene
+ complex as a long-lived ion in an ICR cell has not a classical open structure different from the protonated styrene.
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Hiroshi Abe, Hideaki Nitta, Atsunori Mori, Shohei Inoue
1992 Volume 21 Issue 12 Pages
2443-2446
Published: 1992
Released on J-STAGE: May 15, 2006
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Optically active γ-cyanoallylic alcohols were synthesized by using asymmetric hydrocyanation of α,β-alkenyl aldehydes catalyzed by peptide-titanium complex to give α-cyanoallylic alcohols (cyanohydrins) with high optical yields followed by palladium complex catalyzed [3.3]sigmatropic chirality transfer of the corresponding acetates.
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