一种合成H_2N-Gly-王氏树脂的新工艺

A New Procedure of H_2N-Gly-Wang Resin Synthesis

目的 :本研究旨在建立一种制备 H2 N- Gly-王氏树脂的新工艺 ,提高其结合率。方法 :采用 Fmoc-甘氨酸 :DCC:DMAP:王氏树脂的摩尔比为 10 :5 :1:1,反应时间 1.5 h。 Fmoc-甘氨酸首先与 DCC反应 ,然后加入 DMF使反应中产生的沉淀溶解 ,再加入 DMAP催化 ,使活化的 Fmoc-甘氨酸与羟基树脂缩合 ,生成 Fmoc-甘氨酸 -王氏树脂。当合成产物结合率低于 6 0 % ,可重复这一工艺。结果 :第一轮制备产物的交换当量为 0 .15 m mol/ g,结合率为 31.7% ;第二轮产物的交换当量和结合率分别为 0 .2 7mmol/ g和 5 7.0 8% ;第三轮产物的交换当量及结合率分别是 0 .32 mmol/ g和6 7.6 %。结论 :结果表明 ,该工艺反应时间短 ,第一轮产物的结合率较为满意 ,第二轮、第三轮反应可显著提高产物的结合率。

Objective:To explore a new procedure of H 2N Gly Wang resin to increase the combination rate of the product.Methods:The mole ratio of Fmoc Gly OH:DCC:DMAP:Wang resin was 10∶5∶1∶1,reaction time was 1 5h in this procedure.Firstly,Fmoc Gly OH reacted with DCC,and DMF was added for the dissolution of the precipitated product,and secondly DMAP was added for the esterification of activated Fmoc Gly OH with Wang resin to prepare Fmoc Gly Wang resin.This procedure was repeated when the combination rate of the product was lower than 60%.Results:The substitution and the combination rate of the H 2N Gly Wang resin prepared in first round were 0.15mmol/g and 31.7%,and those in the second round were 0.27mmol/g and 57.08%,and those in the third round were 0.32mmol/g and 67 6% in this procedure,respectively.Conclusion:The short time is spent for this procedure and the substitution and combination rate of the H 2N Gly Wang resin in first round is satisfactory.Furthermore,substitution and combination rate of the products prepared in the second and the third round are increased remarkably in this procedure.