HRID1110191

反应详情

EQUATION

反应方程式

HRID 1110191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.8 ml of 1-chloro-N,N,2-trimethyl-prop-1-enylamine (A. Devos et al., J. Chem. Soc., Chem. Commun., Vol. 1979, p. 1180) is added to a stirred solution of 2.09 g of Fmoc-Asp-OBzl in 20 ml of 1,2-dichloroethane at 0° under an argon atmosphere. After 10 minutes, a solution of 1.2 g of tritylamine in 4 ml of 1,2-dichloroethane is added, and then the mixture is stirred for 2 hours, diluted with ethyl acetate and washed with water. The organic phase is dried and evaporated. The residue is taken up in chloroform and chromatographed on 250 g of silica gel. The fractions containing the Fmoc-Asn(Trt)-OBzl are combined and evaporated; the product is obtained as an amorphous foam.

WORKUP

后处理

  1. washwashed with water
  2. customThe organic phase is dried
  3. customevaporated
  4. customchromatographed on 250 g of silica gel
  5. additionThe fractions containing the Fmoc-Asn(Trt)-OBzl
  6. customevaporated
  7. customthe product is obtained as an amorphous foam