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71.
[reaction: see text] Phosphates from 3-substituted 4,4,4-trifluorobut-2-en-1-ols were found to be effective for construction of CF3-containing quaternary carbon centers by way of Cu(I)-catalyzed Grignard reactions in the presence of catalytic amounts of CuCN and trimethylsilyl chloride (TMSCl) in an anti S(N)2' manner. 相似文献
72.
Abstract— The title aminodioxetane prepared by photooxygenation of 2–(l-methyl-3-indolyl-3-phenyl-1,4-dioxene is fairly stable at ?46°C and gives on warming to room temperature an ultraviolet light at Λmax 320 nm, which corresponds to 377kJ/mol; the highest energy ever observed among the efficient chemiluminescent compounds. The efficiency of chemiluminescence and excited singlet molecule formation in n-hexane were 3.6% and at least 50%, respectively. Substitution and solvent effects suggest polar nature of the transition state as expected from the ‘CIEEL’ mechanism. In polar solvents, the dioxetane gives visible light (Λmax 400 nm in dichloromethane) as well as the UV light; the former being quenched by methanol. This is interpreted in terms of an intramolecular exciplex formation between the indole and phenyl groups. This is the first example of an intramolecular exciplex produced by the dioxetane decomposition. 相似文献
73.
Yuzuru Katagiri Kenzo Kanohta Kazuhiko Nagasawa Tadao Okusa Toshio Sakai Osamu Tsumura Yasuhiko Yotsui 《Analytica chimica acta》1981,133(4):535-543
A practical search system for proton n.m.r. spectra is reported. The coding rules and search algorithms are described in detail. Data for 8000 spectra have been converted into a computer-readable file from printed charts. Several search tests are used to evaluate the usefulness of the search system, and various effects of experimental conditions such as different instruments, frequencies and solvents on recall efficiency are described. The results presented indicate that the system should be applicable to routine analytical work. 相似文献
74.
Oka H Suzuki M Harada K Iwaya M Fujii K Goto T Ito Y Matsumoto H Ito Y 《Journal of chromatography. A》2002,946(1-2):157-162
pH-Zone-refining counter-current chromatography was successfully applied to the separation of the main components of Food Color Red No. 106 (R-106, acid red, Color Index No. 45100). A 300-mg quantity of sample was separated using the following two-phase solvent system: n-butanol-water, 40 mM sulfuric acid in organic stationary phase and 30 mM ammonia in aqueous mobile phase. The obtained fractions were analyzed by high-performance liquid chromatography and fast atom bombardment mass spectrometry. The separation yielded 261.9 mg of main component of acid red with purity of 99.9%. 相似文献
75.
H Harada K Iizuka T Kamijo K Akahane R Yamamoto Y Nakano A Tsubaki T Kubota I Shimaoka H Umeyama 《Chemical & pharmaceutical bulletin》1990,38(11):3042-3047
The experimental details for the synthesis of human renin inhibitors are described. In order to avoid metabolic degradation of the Phe-His (P3-P2) amide bond in transition-state analogs, structurally modified acyl residues (P4-P3) were incorporated into the inhibitors. Compound 1a, which contained 2-(1-naphthylmethyl)-3-(N-phenethylcarbamoyl)propionyl residue (P4-P3) with a retro-inverso amide bond, L-histidine, and norstatine isoamylamide residue (P1-P1) as a transition-state mimic, had potent human renin inhibitory activity, and it lowered blood pressure when administered orally to common marmosets. 相似文献
76.
77.
78.
Fukuji Higashi Shigeru Sugimori Toshio Mashimo 《Journal of polymer science. Part A, Polymer chemistry》1988,26(4):1003-1009
The direct polyesterification with thionyl chloride (SOCl2) in pyridine was further investigated. Copolycondensations of dicarboxylic acids, bisphenols, and hydroxybenzoic acids were significantly affected by the reaction temperatures and combinations of monomers which could change relative rates of alcoholyses of the activated dicarboxylic acids and the hydroxyacids consequently to vary monomer sequences in the copolymers resulted. The sequences were tried to be varied more directly by stepwise reactions of monomers in copolycondensations of dicarboxylic acids, bisphenols, and p-hydroxybenzoic acid (PHB), as well as PHB and m-hydroxybenzoic acid (MHB). The reactions proceeded smoothly and satisfactorily when carried out by initial reaction of dicarboxylic acids and PHB followed by bisphenols likely to favor sequential to random distributions of monomers. Reverse addition of PHB and bisphenols, and then dicarboxylic acids resulted in rapid precipitation due to some oligomerization of PHB at an earlier stage of reaction, and largely retarded the reaction. This was also the case for the copolycondensation of PHB and MHB. Copolymers of high inherent viscosities with up to 65 mol% PHB could be obtained by initial reaction of MHB followed by PHB. 相似文献
79.
Miyazaki A Fujisawa Y Shiotani K Fujita Y Li T Tsuda Y Yokoi T Bryant SD Lazarus LH Okada Y 《Chemical & pharmaceutical bulletin》2005,53(9):1152-1158
1,2-Dihydropyrazin-2-one derivatives, which have two aminoalkyl groups at the positions 3 and 6, were found to be efficient tools for the construction of potent, selective and long-acting opioid mimetics. During the course of preparation, we found that the catalytic hydrogenation of 3,6-bis(benzyloxycarbonylaminomethyl)-5-methyl-1,2-dihydropyrazin-2-one to remove the benzyloxycarbonyl groups resulted in a side reaction. By MS and NMR studies and by preparation of additional 1,2-dihydropyrazin-2-one derivatives, the structure of the by-product was identified as 3-aminomethyl-5,6-dimethyl-1,2-dihydropyrazin-2-one. Preparation of additional compounds substituted with deuterium provided us with sufficient information to confirm the structure of the product and to support a cyclization mechanism in its formation. 相似文献
80.
Structure of an alkaline hydrolysis product of heavenly blue anthocyanin was determined to be -4-0-(6-0-(-3-0-(β-D-glucopyranosyl)caffeyl)-β-D- glucopyranosyl)caffeic acid (). 相似文献