HRID1084991

反应详情

EQUATION

反应方程式

HRID 1084991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

60 mg of [(RS)-4-methyl-2-[[(S)-3-methyl-1-(methylcarbamoyl)butyl]carbamoyl]pentyl](succinimidomethyl)phosphinic acid methyl ester were dissolved in 5 ml of dichloromethane, 0.5 ml of bromotrimethylsilane was added and the mixture was stirred at room temperature for 1.5 hours. The solvent was removed by evaporation and the residue was then re-evaporated twice with 20 ml of acetone and 0.25 ml of water. After standing at room temperature for 15 minutes, the solvent was removed by evaporation and the residue was dissolved in 20 ml of acetone/dichloromethane (1:2). The solution was then evaporated to give 56 mg of [(RS)-4-methyl-2-[[(S)-3-methyl-1-(methylcarbamoyl)butyl]carbamoyl]pentyl](succinimidomethyl)phosphinic acid in the form of a white foam.

WORKUP

后处理

  1. customThe solvent was removed by evaporation
  2. customthe residue was then re-evaporated twice with 20 ml of acetone and 0.25 ml of water
  3. waitAfter standing at room temperature for 15 minutes
  4. customthe solvent was removed by evaporation
  5. dissolutionthe residue was dissolved in 20 ml of acetone/dichloromethane (1:2)
  6. customThe solution was then evaporated