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目的研究并改进松果体素的合成方法.方法以丙烯腈为原料与丙二酸乙酯经Michael反应,所得产物用RaneyNi粉末电极在甲醇介质中以2.5A/dm2的电流密度电催化还原,得到3-羧酸乙酯-2-哌啶酮,再经过重氮化反应,Fischer吲哚化反应,咔啉的开环和脱羧,乙酰化共6步反应,制得N-乙酰基-5-甲氧基色胺.结果与结论电催化还原2-氰基乙基丙二酸二乙酯,获得90%的收率,常压下把腈基还原为胺基,反应避免了高压氢化,合成总收率达到25%.
Objective To study and improve the synthesis of pineal voxel. Methods The reaction of acrylonitrile with ethyl malonate by Michael reaction and the product electrocatalytic reduction with Raney Ni powder electrode in methanol medium at a current density of 2.5 A / dm2 gave ethyl 3-carboxylate-2-piperidine Diketone, diazotization reaction, Fischer indolization reaction, carboline ring opening and decarboxylation, acetylation a total of six-step reaction, N-acetyl-5-methoxy tryptamine. RESULTS AND CONCLUSION Electrocatalytic reduction of diethyl 2-cyanoethylmalonate gave 90% yield. The nitrile group was reduced to an amine group at atmospheric pressure, and the high pressure hydrogenation was avoided. The overall yield was 25% .