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作 者:杨艺虹[1] 吴元欣[1] 杨建设[1] 李培成[2] 张珩[1]
机构地区:[1]武汉化工学院,湖北武汉430073 [2]武汉化工研究所,湖北武汉430074
出 处:《精细化工中间体》2004年第2期19-21,共3页Fine Chemical Intermediates
摘 要:采用不对称转换法制备D( ) 对羟基苯甘氨酸(D( ) HPG)。DL(±) HPG在醋酸溶剂中,以甲苯磺酸(TS)为拆分剂,在苯甲醛的催化下制得D( ) HPG·TS盐,讨论了催化剂的用量、反应温度及反应时间对收率的影响,确定最佳工艺条件为:DL HPG∶TS∶苯甲醛=1∶1 025∶0 1(mol),反应温度100℃,反应时间6h。然后用氨水调pH至5~6得D( ) HPG。总收率为77 3%,光学纯度为98 9%。D(-)-4-hydroxyphenylglycine (D(-)-HPG) was prepared by the method of asymmetric transformation. D(-)-HPG·TS salts was obtained by reaction of DL (±)-HPG with TS in acetic acid in the presence of small amounts of benzaldehyde. The influences on catalyst dosage, temperature and time were discussed. Th optimum technological conditions are as follow: DL-HPG∶TS∶benzaldehyde=1∶1.025∶0.1(mol), reaction temperature 100℃ and reaction time 6h. D(-)-HPG was obtained by neutralisation to pH5~6 with ammonia. The overall yield is 77.3% and optical purity 98.9%.
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