2-(3-(呋喃-2-基)丙烯酰胺基)3-苯基丙酸的制备工艺研究

Preparation of 2-(3-(Furan-2-yl)acrylamide) 3-phenylpropionic Acid

以2-呋喃丙烯酸和L-苯丙氨酸甲酯盐酸盐为原料制备了2-(3-(呋喃-2-基)丙烯酰胺基)3-苯基丙酸()。并优化了中间体3-(2-呋喃基)丙烯酰基-L-苯丙氨酸甲酯()工艺条件。优化条件为:反应温度5℃,原料n(2-呋喃丙烯酸)∶n(L-苯丙氨酸甲酯盐酸盐)∶n(苯并三氮唑-1-基氧基三(二甲基氨基)磷鎓六氟磷酸盐(BOP)=0.90∶1.00∶2.00,反应溶剂二氯甲烷,反应时间20 h;水解得的适宜温度为20℃,总收率为87.53%,纯度为98.55%。工艺收率高、成本低,适合工业化生产。

2-(3-(Furan-2-yl)acrylamide)3-phenylpropionicacid() was prepared using 2-furanacrylic acid and L-phenylalanine methyl ester hydrochloride as raw materials. The optimum process conditions were obtained after experimental evaluation as followings: preparation of 3-(2-furanyl)acryloyl-l-phenylalanine methyl ester() at reaction temperature of 5 ℃,the material ratio of 2-furanacrylic acid to L-phenylalanine methyl ester hydrochloride and BOP of 0.90 ∶1.00∶2.00, dichloromethane as reaction solvent, reaction time of 20 h;the optimum temperature for hydrolysis of 20℃, the yield of is 87.53% with apurity of 98.55%. This process had the advandages including lower cost and high yield. It was suitable for industrial production.