摘要
以4-氯苯甲醛、丙二酸为起始原料,以氨气为氨化剂在高压釜内反应得目标产物3-氨基-3-(4-氯苯基)丙酸.研究了工艺条件对反应的影响.其适宜的合成工艺条件:在反应温度95℃,氨气压力控制在0.6～0.8MPa下,选用乙醇为溶剂,哌啶为催化剂,催化剂用量为5％(质量分数),4-氯苯甲醛和丙二酸的物质的量比为1∶1.4,反应10h,收率可达79.4％,产品熔点为222.5～222.7℃.该方法以氨气为氮化剂不仅原料成本比乙酸铵低,而且产品纯度也更高,更容易实现大规模工业化生产.
3-amino-3-(4-chlorophenyl)propionic acid was prepared in autoclave using 4-chlorobenzaldehyde and malonic acid as raw materials,and ammonia as ammoniating agent.The effect of reaction conditions on reaction was studied.It has been shown that the yield of 3-amino-3-(4-chlorophenyl)propionic acid can be up to 79.4%under reaction temperature 95℃,reaction time 10h and the molar ratio of 4-chlorobenzaldehyde to malonic acid being 1∶1.4,using ethanol as solvent,piperidine as catalyst,the amount of catalyst being 5%,ammonia pressure in the range of 0.6~0.8MPa,the melting point of product is 222.5~ 222.7℃.The cost of ammonia as ammoniating agent in this method is lower than ammonium acetate,and the purity of the product is also higher,so it is easy to implement large-scale industrial production.
出处
《常州大学学报（自然科学版）》
CAS
2014年第1期28-31,共4页
Journal of Changzhou University：Natural Science Edition
