【摘要】 以噻吩和3-氯丙酰氯为原料,经傅克反应生成3-氯-1-(2-噻吩)-丙酮,用硼氢化钠加氢还原得到混旋的度洛西汀中间体3-氯-1-(2-噻吩)-丙醇中间体。利用D-扁桃酸为拆分剂对其中间体进行手性拆分得到较纯的(S)-3-氯-1-(2-噻吩)-丙醇。实验结果表明,3-氯-1-(2-噻吩)-丙醇与D-扁桃酸摩尔的量的比值为主要因素,析出晶体温度和溶剂为次要因素。以苯为溶剂时,3-氯-1-(2-噻吩)-丙醇与D-扁桃酸的量的摩尔比值为1∶0.4,析出温度为0℃,拆分效果较好,其o.p.值为74%。更多还原

【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 %.更多还原