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21.
The Pictet-Spengler cyclization of the imines (3) prepared by the condensation of L-tryptophan methyl ester (1) and aryl methyl ketones (2), using titanium(IV) isopropoxide as an iminating reagent, quantitatively proceeded, when treated with trifluoroacetic acid (TFA) or formic acid, to provide two diastereomers, that is (1S,3S)-1-aryl-3-isopropoxycarbonyl-1-methyl-1,2,3,4-tetrahydro-beta-carbolines (4) and their (1R,3S)-diastereomers (5), of which the diastereomer ratios varied from 1 to 5 depending on the reaction conditions. The (1R,3S)-diastereomers (5) are thermodynamically more stable than their (1S,3S)-congeners (4), as shown by equilibration experiments in TFA. The conversion of 4 to 5 (also 5 to 4) should occur under acidic conditions by cleavage of the C(1)-N(2) bond with complete retention of configuration at the C-3 chiral center. The low diastereo-selectivity observed in the Pictet-Spengler reaction of 1 and 2 is concluded to be a stereochemical outcome under conditions of kinetic control (lower temperature, shorter reaction time), while the high diastereo selectivity with preferential formation of the more stable isomer (5) is the result of thermodynamically controlled experiments (higher temperature, longer reaction time). 相似文献
22.
Tetsuji Kametani Kazuo Kigasawa Mineharu Hüragi Nagatoshi Wagatsuma Setsu Saitoh Hideo Sugi 《Journal of heterocyclic chemistry》1973,10(3):313-315
Acid treatment of the alkylated products of (Va, Vb, and VIII) of piperidinols IVa and IVb, and tetrahydropyridine VII with β-bromoethylbenzene, afforded 1,2,3,4,5,6-hexahydro-8-hydroxy-2,6-methano-6,1 1-dimethyl-3-phenethyl-3-benzazocine (la) in good yield. Piperidinols Va and Vb were also obtained from the reaction of N-(3-methyl-3-pentenyl)-β-phenethylamine (IIb) with methyl 3-(4-methoxyphenyl)-2,3-epoxypropionate. 相似文献
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24.
Akihiko Ishii Masashi Saitoh Tetsuhiko Kawai Masami Murata Juzo Nakayama 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8-9):2025-2026
The reaction of isolable dithiirane 1-oxides with (Ph 3 P) 2 Pt( m 2 -C 2 H 4 ) provided the title complexes in high yields. 31 P NMR spectroscopy of the phosphine ligands of the complexes and x-ray crystallographic analysis of a complex were reported. 相似文献
25.
M. Igarashi K. KakimotoT. Hayashida Y. HanadaS. Fujita K. MoritaN. Nakamura S. HanyuY. Sutoh H. KutamiY. Iijima T. Saitoh 《Physica C: Superconductivity and its Applications》2010,470(20):1230-1233
We have studied a hot-wall heating system to produce GdBa2Cu3Oy (GdBCO) films with large critical currents (Ic) at a high production rate by a pulsed-laser-deposition (PLD) method. GdBCO films fabricated at a production rate of 30 m/h under the optimized conditions, especially a distance of 95 mm between the target and the substrate (T–S), exhibited high critical current densities (Jc) of about 3 MA/cm2 and Ic over 300 A at a thickness of 1–2 μm. Furthermore, long GdBCO tapes prepared by repeated depositions at each tape-passing speed of 80 m/h showed uniform Ic distribution along the longitudinal direction, because the hot-wall system enabled to stabilize temperature within a few degrees at 800 °C. A 170 m long tape with Ic over 600 A was successfully fabricated at a production rate of 16 m/h using a laser power of 360 W. 相似文献
26.
Hiroyuki Nishide Naoki Yoshioka Yukoh Saitoh Ritsuko Gotoh Takeshi Miyakawa Eishun Tsuchida 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(9):775-786
Abstract m- and p Bis(diphenylene)propenylphenylacetylene (m-, p-8) were synthesized and polymerized with WCI6, MoCl5, and Rh catalyst, yielding solvent-soluble poly(phenylacetylene)s bearing a π-conjugated bis(di-phenylene)propenyl groups (m-, p-7a). The polymers gave their polyanion derivatives, which were electrolytically and chemically oxidized to yield the corresponding polyradicals (m-, p-7b). The polyradicals were chemically very stable due to the resonance stabilization of an unpaired electron whose spin concentration could be increased up to ca. 2 × 1023 spins per molar monomer unit. ESR spectroscopy suggested an antiferro-magnetic interaction between unpaired electrons. 相似文献
27.
The molecular aggregation of acrylic and methacrylic acid esters containing long-fluorocarbon chains: 2-(perfluoroalkyl)ethyl acrylate (FFnEA) and 2-(perfluoroalkyl)ethyl methacrylate (FFnEMA) (F(CF2)nCH2CH2OCOC(X)=CH2, where X=H, CH3 and n=6, 8, 10) was investigated by differential scanning calorimetry (DSC) and temperature controlled X-ray powder diffraction measurement. These compounds exhibited some characteristic polymorphic behaviors depending on the length of fluorocarbon chain and the -position methyl group. The solid-state polymerization by -ray irradiation was studied for these compounds in the various crystal forms. In the solid-state polymerization, highest polymerizability was observed in the crystal form that exists in the highest temperature region for each compound.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
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29.
Photochemical vapor deposition of a-Si films at a high rate using SiH4 and a 185 nm low pressure mercury lamp is described. A maximum rate of 1 nm/sec was attained using the 185 nm lamp. This rate was about ten times higher than that using a 254 nm lamp. Assuming that there is no interaction between the effects of the two wavelengths, the deposition rate per light output power of 184.9 nm light is 160 times larger than that for 253.7 nm light. The absorption cross-section of the 184.9 nm light is ten times greater than that for the 253.7 nm light. 相似文献
30.
Kakuyanagi K Saitoh M Kumagai K Takashima S Nohara M Takagi H Matsuda Y 《Physical review letters》2005,94(4):047602
We present a 115In NMR study of the quasi-two-dimensional heavy-fermion superconductor CeCoIn5 believed to host a Fulde-Ferrel-Larkin-Ovchinnikov (FFLO) state. In the vicinity of the upper critical field and with a magnetic field applied parallel to the ab plane, the NMR spectrum exhibits a dramatic change below T*(H) which well coincides with the position of reported anomalies in specific heat and ultrasound velocity. We argue that our results provide the first microscopic evidence for the occurrence of a spatially modulated superconducting order parameter expected in a FFLO state. The NMR spectrum also implies an anomalous electronic structure of vortex cores. 相似文献