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帕珠沙星注册杂质合成研究

时间:2018-04-12 13:45来源:毕业论文
以P-2为原料,选用DMF(二甲基甲酰胺)为反应溶剂,选用2.0当量的固体氰化钠,温度控制在80±2℃,搅拌下反应时间为10小时,不添加碱
摘要:帕珠沙星是目前市场上广泛应用的第四代喹诺酮类抗菌药,本论文分析了其生产工艺中可能出现的两种杂质,并制订了一系列合成几种杂质的化学方法。得到适量的样品,为下一步的科学研究提供原料和依据。对各反应阶段的溶剂、反应物当量和当量、反应温度、反应添加剂的形式和当量以及反应体系等反应条件进行优化研究,选择出最佳的工艺条件。B-4((S)-9-氟-10-(1-乙酰亚胺基环丙基)-3-甲基-2,3-二氢-7-氧代-7H-吡啶并[1,2,3-de] [1,4]苯并恶嗪-6-羧酸):以帕珠沙星为原料,选用吡啶为反应溶剂,选用6.0当量的乙酸酐,温度控制在60±2 ℃,搅拌下反应时间为16小时,按此条件实验,B-4产率最优可达80.6%。P-3((S)-9-氟-10-羧基-3-甲基-2,3-二氢-7-氧代-7H-吡啶并[1,2,3-de] [1,4]苯并恶嗪-6-羧酸乙酯):以P-2为原料,选用DMF(二甲基甲酰胺)为反应溶剂,选用2.0当量的固体氰化钠,温度控制在80±2℃,搅拌下反应时间为10小时,不添加碱,按此条件实验,P-3产率最优可达60.3%。D-9((S)-9-氟-10-羧基-3-甲基-2,3-二氢-7-氧代-7H-吡啶并[1,2,3-de] [1,4]苯并恶嗪-6-羧酸):以P-3为原料,使用乙醇为反应溶剂,选用NaOH溶液(1mol/L,5.0当量),温度控制在90±2℃~100±2℃,搅拌下反应时间为5小时,按此条件实验,D-9产率最优可达89.3%。21001
重庆时时彩的规律关键词:帕珠沙星;合成;当量;B-4;P-3;D-9
Sign Pazufloxacin synthesis of impurities
Abstract: pazufloxacin is now widely used on the market fourth generation quinolone antibacterial drugs, this paper analyzes two kinds of impurities may arise in production process, and established a series of chemical method synthesis of several impurities. Get the right amount of samples, to provide raw materials and the scientific basis for the next step research. The reaction solvent, reactant equivalent and equivalent, reaction temperature, additives and equivalent and reaction system and the reaction condition were studied, the optimum process conditions of choice. B-4 ((S) -9- -10- (f 1- acetyl imine cyclopropyl) -3- methyl -2,3- two hydrogen -7- oxo -7H- pyridine and [1,2,3-de] [1,4] benzoxazine -6- carboxylic acid): pazufloxacin as raw material, using pyridine as solvent, acetic anhydride using 6 equivalent, temperature control at 60 ± 2 ℃, stirring reaction time is 16 hours, the experiment according to these conditions, the yield of B-4 optimal up to 80.6%. P-3 ((S) -9- -3- -2,3- two fluoro -10- carboxyl methyl hydrogen -7- oxo -7H- pyridine and [1,2,3-de] [1,4] benzoxazine -6- carboxylic acid ethyl ester): with P-2 as raw material, using DMF (two methyl formamide) as a reaction solvent, solid sodium cyanide with 2 equivalent, temperature control at 80 ± 2 ℃, mixing reaction time mix for 10 hours, do not add alkali, the experiments according to this condition, the yield of P-3 optimal up to 60.3%. D-9 ((S) -9- -3- -2,3- two fluoro -10- carboxyl methyl hydrogen -7- oxo -7H- pyridine and [1,2,3-de] [1,4] benzoxazine -6- carboxylic acid): with P-3 as raw material, the use of ethanol as solvent, using NaOH solution (1mol/L, 5 equivalents), temperature 2 ℃ ~100 ± 2 ℃ at 90 ±, stirring under the reaction time of 5 hours, the experiment according to these conditions, the yield of D-9 optimal up to 89.3%.
源自~六%维^论*文-网).加7位QQ3249'114 重庆时时彩的规律 www.mamitama.com

Keywords: Paper Shah Singh; synthesis; equivalence; B-; P-3; D-9
目录
1 绪论    1
1.1 本课题国内外研究现状概述    1
1.1.1 甲磺酸帕珠沙星简介    1
1.1.2 帕珠沙星合成工艺    1
1.1.3 帕珠沙星的抗菌机制及优势    2
1.2 喹诺酮类药物    3
1.2.1 喹诺酮药物概述    3
1.3 合成实验中常用提纯方法和检测方法    4
1.3.1 减压蒸馏    4 帕珠沙星注册杂质合成研究:重庆时时彩的规律/a/huaxue/20180412/12993.html
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