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本文报道4-甲基戊醛(4)的吗啉烯胺和甲基乙烯基酮反应,然后水解得4-异丁基环己酮异构体混合物,后者和2-溴代丙酸乙酯进行Reformatsky反应,芳构化、水解得布洛芬(11)的方法。异戊基溴化镁(1)和二甲基甲酰胺缩合得粘稠的镁盐络合物(2),室温搅拌72小时后,用3N盐酸处理得4-甲基戊醛(4)。4经常规法与吗啉反应得吗啉烯胺5,继而和甲基乙烯基酮在无水乙醚中缩合,得4-异丁基环己基-2-烯-1-酮(6)和4-异丁基环己基-3-烯-1-酮(7)的混合物,经气液色谱分析6/7=70/30。该混合物和锌粉、2-溴代丙酸乙酯反
It is reported herein that morpholine enamine of 4-methylpentanal (4) is reacted with methyl vinyl ketone and then hydrolyzed to give a mixture of 4-isobutyl cyclohexanone isomers, the latter being reacted with ethyl 2-bromopropionate Reformatsky reaction, aromatization, hydrolysis of ibuprofen (11) method. Isoamylmagnesium bromide (1) and dimethylformamide were condensed to give a viscous magnesium salt complex (2). After stirring at room temperature for 72 hours, 4N-methylpentanal (4) was treated with 3N hydrochloric acid. 4 conventional method morpholine reaction with morpholine enamine 5, and then with methyl vinyl ketone in anhydrous ether to give 4-isobutyl cyclohexyl 2-en-1-one (6) and 4-iso Butylcyclohexyl-3-en-1-one (7) was analyzed by gas liquid chromatography with 6/7 = 70/30. The mixture was reacted with zinc powder, ethyl 2-bromopropionate