Liu Yan-me
2014
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Journal
Technology & Development of Chemical Industry
Abstract
Starting from thiophene and 3-chloropropinylchloride, 3-chloro-1-(2-thienyl)propanone was prepared by Friedel-Crafts reaction. Then using sodium borohydride, 3-chloro-1-(2-thienyl)propanol was prepared through hydrogenation reduction. Through chiral separation, the relatively pure product(S)-3-chloro-1-(2-thienyl)propanol was got. The results of experiment indica ted that the molar ratio of 3-chloro-1-(2-thienyl)propanol to D-(-)-mandelic acid was the main factor, and the crystallized temperature and the solvent were secondary factors. When the solvent was benzene and the molar ratio of D-(-)-mandelic acid to 3-chloro-1-(2-thienyl) propanol was 0.4 : 1, the crystallized temperature was 0℃, the better results of separation was got, the value of o.p.(optical purity) was 74 %.