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以(S)-10-氰甲基-9-氟-3-甲基-7-氧代-3,7-二氢-2H-[1,4]-口恶嗪[2,3,4-ij]喹啉-6-羧酸乙酯(Ⅱ)为原料,经环合、水解“一锅法”反应,制备帕珠沙星高级中间体(S)-10-(1-环丙基甲酰胺)-9-氟-3-甲基-7-氧代-3,7-二氢-2H-[1,4]-口恶嗪[2,3,4-ij]喹啉-6-羧酸(Ⅳ),探讨了温度、碱、溶剂等对反应的影响。确定较佳的合成工艺条件为:n(化合物Ⅱ):n(1,2-二氯乙烷):n(苄基三乙基氯化铵):n(氢氧化钠)=1:1.5:0.43:16.7,水作为溶剂,先室温搅拌5 h,随后加热到70℃反应2 h,收率达82%。
(S) -10-cyanomethyl-9-fluoro-3-methyl-7-oxo-3,7-dihydro-2H- [1, 4] -oxazin [2,3,4- ij] quinoline-6-carboxylic acid ethyl ester (Ⅱ) as raw materials, cyclization, hydrolysis “one pot ” reaction to prepare pazufloxacin higher intermediate (S) -10- Yl) carbamate) -9-Fluoro-3-methyl-7-oxo-3,7-dihydro-2H- [1,4] oxazin [2,3,4-ij] - carboxylic acid (Ⅳ), to explore the temperature, alkali, solvents and other effects on the reaction. The best synthesis conditions are: n (compound Ⅱ): n (1,2-dichloroethane): n (benzyltriethylammonium chloride): n (sodium hydroxide) = 1: 1.5: 0.43: 16.7, water as a solvent, first stirred at room temperature for 5 h, then heated to 70 ℃ for 2 h, the yield was 82%.