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以环戊酮、环己酮和吗啉为起始原料,以磺酸凝胶树脂732为催化剂,分别合成了环戊基吗啉烯胺和环己基吗啉烯胺,然后选择叔丁醇为溶剂,环戊(己)基吗啉烯胺和丙烯酸甲酯进行迈克尔加成反应,生成环戊(己)酮-2-(β-)丙酸甲酯,经钯碳和硫酸还原酮羰基,脱水,水解生成3-环戊(己)基丙酸。主要考察了反应过程中催化剂和溶剂对产品合成工艺的影响。结果表明,以吗啉为有机胺利用磺酸凝胶树脂催化合成烯胺化合物,工艺简单,烯胺收率达98%以上;在迈克尓加成反应中,选用叔丁醇为溶剂,收率达95%以上,溶剂可回收利用;最后采用钯碳和硫酸进行还原反应,产品收率达85%以上。
Cyclopentanone, cyclohexanone and morpholine were used as starting materials and sulfogel resin 732 was used as a catalyst to synthesize cyclopentyl morpholine enamine and cyclohexyl morpholine enamine, respectively, then tert-butanol was selected as Solvent, cyclopentyl (hexyl) morpholineenamine, and methyl acrylate to form methyl cyclopentanone 2- (β-propionate, reduction of the ketone carbonyl group with palladium carbon and sulfuric acid, Dehydration, hydrolysis 3-cyclopentyl (hexyl) propionic acid. Mainly investigated the reaction of the catalyst and solvent on the product synthesis process. The results showed that morpholine as organic amine sulfonate gel resin catalyzed synthesis of enamine compounds, the process is simple, the yield of enamine reached 98% or more; in the Michael addition reaction, the choice of tert-butyl alcohol as the solvent, the yield Up to 95%, the solvent can be recycled; Finally, the use of palladium carbon and sulfuric acid reduction reaction, the product yield of 85% or more.