Abstract: In this paper, the cyclopentanone, cyclohexanone and morpholine were used as the starting materials and sulfonylurea gel resin732 as catalysts to synthesize enamine. Then tertiary butanol was selected as organic solvent. Micheal addition was operated between enamines and methyl acrylate to synthesize Cyclopentanone-2-(- β)methyl propionate and Cyclohexanone-2-(-β)methyl propionate. And then the carbonyl were reduced, dehydrated by palladium carbon and sulfuric acid to the 3-Cyclopentylpropionic acid and 3-Abstract: In this paper, the cyclopentanone, cyclohexanone and morpholine were used as the starting materials and sulfonylurea gel resin732 as catalysts to synthesize enamine. Then tertiary butanol was selected as organic solvent. Micheal addition was operated between enamines and methyl acrylate to synthesize Cyclopentanone-2-(- β)methyl propionate and Cyclohexanone-2-(-β)methyl propionate. And then the carbonyl were reduced, dehydrated by palladium carbon and sulfuric acid to the 3-Cyclopentylpropionic acid and 3-Cyclohexylpropionic acid. During the course, the effect of the catalysts and solvent were investigated. The results showed that the synthetic process of enamine with morpholine as raw material and sulfonylurea gel resin as catalysts is facility, and the yield of the product can up to 98%. In the following reaction in which t-butyl alcohol was applied as solvent, the yield can reach to 95%, and moreover, the solvent can be recycled. In the final reduction reactions with palladium carbon and sulfuric acid as the reducing agent, the yield of 3-Cycloalkylpropionic acid can reach to 85%.