小分子多肽合成方法的改进

AMELIORATION OF THE SYNTHETIC METHOD OF SMALL POLYPEPTIDES AND ITS APPLICATION

采用三苯氯甲烷替代三苯甲醇 ,以 BF3· Et2 O作为催化剂保护巯基 ,产率明显提高(72 %～ 95% ) ;采用乙腈的水溶液作为反应体系 ,控制投料温度 ,活泼酯与氨基酸能顺利结合 ,产率普遍达到 85% ,节省了原料 ,并大大简化了实验操作 .利用上述改进方法成功地合成了有潜在药用前景的新手性小分子多肽 ,其结构得到了严格的谱学鉴定 ,经过了 IR,!HNMR,1 3CNMR,MS或元素分析的确证 .

Using triphenylchloromethane instead of triphenylmethano l and taking boron trifluoride etherate as catalyst, the protection of mer capto group can be successfully performed, whose yield is increased from 72% to 95%. Active ester can easily rea ct with amino acids in the mixed solvents of acetonitrile and water according to decent beginning temperature so that materials are saved and the procedure is s implified. All of the yields are above 85%. Several small polypeptides with nove l chiral center and talent medical prospect are synthesized employing the proced ure above, all of which are identified on the basis of their analytic data and s pectroscopic data such as IR,1HNMR,13CNMR and MS.