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以异戊醛和氰基乙酸乙酯为原料,经Knoevenagel缩合、氰基加成、高温脱羧3步反应合成了普瑞巴林中间体异丁基丁二腈(Ⅲ),其中第1步和第2步反应产物分别为5-甲基-2-氰基-2-己烯酸乙酯(Ⅰ)和5-甲基-2,3-二氰基己酸乙酯(Ⅱ)。通过对原料配比、反应温度、反应时间等反应条件的考察和优化,得到最优反应条件下化合物Ⅰ、Ⅱ、Ⅲ的收率分别达到92.3%、93.6%和94.2%,总收率为81.4%。各反应产物的结构通过1HNMR、IR及MS进行了表征和确认。
An isobutyl succinonitrile (Ⅲ) was synthesized from isobutyraldehyde and ethyl cyanoacetate by Knoevenagel condensation, cyano addition and high temperature decarboxylation. The first and the second The 2-step reaction products were ethyl 5-methyl-2-cyano-2-hexenoate (I) and ethyl 5-methyl-2,3-dicyanohexanoate (II). Through the investigation and optimization of reaction conditions, such as the ratio of raw materials, reaction temperature and reaction time, the yields of compounds I, II and III reached 92.3%, 93.6% and 94.2% under the optimum reaction conditions respectively. The total yield was 81.4 %. The structure of each reaction product was characterized and confirmed by 1HNMR, IR and MS.