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Qingmin Wang Runqiu Huang 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):173-179
Abstract 1-Oxo-4-chlorocarbony1-1-phospha-2,6,7-trioxabicyclo[2.2.2]octane (5) was obtained from phosphorus oxychloride. Benzyl chloroformate was synthesized by the reaction of benzyl alcohol and triphosgene in good yield for the first time. N-r-Butyl-N-benzoylhydrazine(II) was prepared in a new and convenivent procedure with good yield. The reaction of 5 and II proceeded smoothly in the presence of sodium carbonate and afforded the desired compound 13 in good yield, while in the presence of triethylamine, the elimination of butyl was observed and afforded the compound 12. 相似文献
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Zhanxiang Liu Zhaosheng Song Jinlong Zhao Jianyong Zheng 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2375-2381
A highly efficient, solid-phase synthesis of 2-arylamino-5-(4-hydroxy-phenyl)-1,3,4-thiadiazole derivatives under mild conditions has been developed. The 1,3,4-thiadiazole derivatives were synthesized from resin-bound acylhydrazines in several steps, which gave 78–88% overall yields and excellent purities of the products. 相似文献
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Diacylhydrazines have been found as molting hormone analogs since RH‐5849 was reported as the first nonsteroidal ecdysone agonist in 1988. Optimizations on diacylhydrizines with benzoheterocycle containing oxygen were widely explored in recent years. In order to find novel compounds with high bioactivity, a series of mono‐ ( I ) and di‐acylhydrazine ( II ) derivatives containing furan were designed and synthesized. Their structures were confirmed by 1H NMR, IR, elemental analyses and single crystal X‐ray diffraction analyses ( II 7). The bioassay results showed that some of the mono‐acylhydrazine ( I ) derivatives exhibited good larvicidal activity against Culex pipiens pallens at 10 mg/L and better than those of di‐acylhydrazines ( II ). Generally, the anti‐tumor activity of di‐acylhydrazines ( II ) was better than that of mono‐acylhydrazines ( I ). 相似文献
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Solid-phase synthesis of aryl, heteroaryl, and sterically hindered alkyl amines using the Curtius rearrangement 总被引:1,自引:0,他引:1
An efficient method for the solid-phase synthesis of aryl amines, heteroaryl amines, and sterically hindered alkyl amines has been developed. The key step in this process was the formation of resin-bound carbamates (B) by the Curtius rearrangement of aryl carboxylic acids with Wang resin providing the trapping hydroxyl group. N-Alkylation reactions of B gave secondary amines in good yield. Some biaryl amines, which are found widely in biologically active substances, were also prepared by the Suzuki reaction of resin-bound carbamates of 2-iodoaniline (16) or 3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (21). The developed methods can be applied to the preparation of libraries containing aryl, heteroaryl, and sterically hindered alkyl amine structures as the pharmacophores. 相似文献
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Highly efficient solid-phase synthesis of 4,5-disubstituted-1,2,4-triazole-3-thiones under mild conditions has been developed. 4,5-Disubstituted-1,2,4-triazole-3-thione derivatives were synthesized from resin-bound acylhydrazines in several steps, providing 76–89% overall yields and excellent purity. 相似文献
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以萘二甲酰亚胺与罗丹明B酰肼基硫脲两种有机荧光染料的光谱重叠特性, 及罗丹明B酰肼基硫脲在pH诱导下的可逆“开-闭”环反应为基础, 分别将其作为荧光共振能量转移(Fluorescence Resonance Energy Transfer, FRET)体系的供、受体, 并与聚N-异丙基丙烯酰胺(PNIPAM)的温敏特性相结合, 通过一系列化学反应, 合成了一种具有双重荧光刺激-响应特性的大分子P(NIPAM-co-RhBHA)-NP. 采用1H NMR、FTIR、UV-vis和GPC对其结构进行了表征. 采用荧光光谱(PL)研究了缓冲溶液中该聚合物对环境温度和pH值的双重荧光响应行为, 并对其影响机制进行了探讨. 结果表明, 酸性条件下大分子中RhBHA和NP-NH2之间会发生荧光共振能量传递; pH值和环境温度变化对大分子P(NIPAM-co-RhBHA)-NP的荧光发射具有显著影响. 相似文献
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Six diaryl acylhydrazine compounds were synthesized in normal temperature with self-made acyl-diazene compounds as raw materials and NH_2NH_2·H_2O as reducer.The products were confirmed by means of elemental analysis,IR and~1H NMR.In the results of IR,there were two N-H absorption at approximately 3200 and 3400 cm~(-1).However,the absorptions of N=N in raw materials disappeared.In the results of 1H NMR,the N-H chemical shifts couldn't be found.Meanwhile,two N-H chemical shifts were detected about from 8.46 to 11.38,respectively.The results of products' elemental analysis were consistent with the theoretical values.The yields of those six products were about from 84% to 93%. 相似文献
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《合成通讯》2013,43(22):3953-3960
Abstract The resin-bound bismethylthiomethylene cyclic malonic acid ester 3 was built up efficiently. Resin 3 can react with arylamines and subsequent thermal cyclizations give 2-alkylthio-4-(1H)-quinolones. Furthermore, conjugate addition of Grignard reagents to the resin 3 forms the resin 6 which was reacted with aryl amines and subsequent thermal-cyclization-cleavages afford the 2-alkyl-4-(1H)-quinolones. 相似文献