HRID1060436

反应详情

EQUATION

反应方程式

HRID 1060436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-(2,6-Dichlorobenzoyl)-4-(4-allylamino-2,6-dimethoxyphenyl)-L-phenylalanine methyl ester (0.93 g) was dissolved in MeCN/water (40 mL of 84:16) under N2. Wilkinson's catalyst (79 mg ) was added and the mixture was brought to boiling. After 2 h, more catalyst (170 mg ) was added and the reaction continued for another 6 h. The solvent was evaporated and the residual water coevaporated with MeCN. The residue was purified by preparative TLC (silica gel; eluent: hexane/AcOEt 2:1 to 1:2) to give N-(2,6-dichlorobenzoyl)-4-(4-amino-2,6-dimethoxyphenyl)-L-phenylalanine methyl ester(708 mg).

WORKUP

后处理

  1. waitthe reaction continued for another 6 h
  2. customThe solvent was evaporated
  3. customThe residue was purified by preparative TLC (silica gel; eluent: hexane/AcOEt 2:1 to 1:2)