摘要
以(R)-(-)-3-氯-1,2-丙二醇为原料合成了医药中间体(R)-(-)-3-氯-2-羟丙基对甲苯磺酸酯,探讨了反应温度、反应时间、溶剂种类及用量、催化剂种类及用量,以及原料配比等因素对反应的影响。通过正交试验确定了适宜的合成工艺条件:反应温度0℃;反应时间6 h;对甲苯磺酰氯与(R)-(-)-3-氯-1,2-丙二醇摩尔比为1.2∶1;催化剂NaOH与(R)-(-)-3-氯-1,2-丙二醇的摩尔比为1.2∶1;以乙酸乙酯为溶剂,(R)-(-)-3-氯-1,2-丙二醇浓度为125 g/L。在此工艺条件下产物得率大于85%。
Synthesis of the medicinal intermediate （R）-（-）-3-chloro-2-hydroxypropyl tosylate was carried out by the reaction of （R）-（-）-3-chloro-1,2-propanediol and p-toluenesulfonyl chloride in this paper. The influences of the reaction temperature, reaction time, type and dosage of solvent, type and dosage of catalyst, and （R）- （-）-3-chloro-1,2-propanediol/p-toluenesulfonyl chloride ratio on the selectivity of esterification and yield of product were investigated. The suitable synthesis conditions were obtained by optimization with orthogonal experiments： reaction temperature 0℃, reaction time 6 h, the molar ratio of p-toluenesulfonyl chloride to （R）-（-）-3-chloro-1,2-propanediol 1.2：1, the molar ratio of catalyst NaOH to （R）-（-）-3-chloro-1,2-propanediol 1.2： 1. Ethyl acetate was used as solvent, and the concentration of （R）-（-）-3-chloro-1,2-propanediol was 125 g/L. The yield of （R）-（-）-3-chloro-2- hydroxypropyl tosylate was over 85 %.
出处
《南京林业大学学报（自然科学版）》
CAS
CSCD
北大核心
2007年第6期34-38,共5页
Journal of Nanjing Forestry University：Natural Sciences Edition
