HRID476697

反应详情

EQUATION

反应方程式

HRID 476697 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 each time. The residue was dissolved in 5 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 each time
  3. dissolutionThe residue was dissolved in 5 ml of acetone
  4. waitAfter standing at room temperature for 15 minutes
  5. customthe solvent was removed by evaporation
  6. dissolutionthe residue was dissolved in 20 ml of acetone/dichloromethane (1:2)
  7. customThe solution was then evaporated