论文部分内容阅读
对羟基苯甲醛在碳酸钾存在下与溴代异丁烷成醚生成4-(2-甲基丙氧基)苯甲醛,与溴素反应生成3-溴-4-(2-甲基丙氧基)苯甲醛,与盐酸羟胺经肟化反应生成3-溴-4-(2-甲基丙氧基)苯甲醛肟,在乙腈中经氯化亚砜脱水生成3-溴-4-(2-甲基丙氧基)苄腈,在三乙胺存在下与硫化铵溶液反应生成3-溴-4-(2-甲基丙氧基)苯甲硫代酰胺,在无水乙醇中与α-氯乙酰乙酸乙酯反应生成2-[3-溴-4-(2-甲基丙氧基)苯基]-4-甲基-5-噻唑甲酸乙酯,再与氰化亚铜反应后水解制得非布索坦,总收率为41%。
Synthesis of 4- (2-methylpropoxy) benzaldehyde from p-hydroxybenzaldehyde with bromoisobutane in the presence of potassium carbonate and reaction with bromine to form 3-bromo-4- (2-methylpropoxy) benzaldehyde oxime by hydroxylation with hydroxylamine hydrochloride, and dehydrated in thionyl chloride with acetonitrile to form 3-bromo-4- (2 - methylpropoxy) benzonitrile is reacted with ammonium sulphide solution in the presence of triethylamine to give 3-bromo-4- (2-methylpropoxy) benzothioamide in anhydrous ethanol with α - ethyl chloroacetoacetate to form ethyl 2- [3-bromo-4- (2-methylpropoxy) phenyl] -4-methyl-5-thiazolecarboxylate, which is reacted with cuprous cyanide Hydrolysis of febuxostat, the total yield was 41%.