HRID476694

反应详情

EQUATION

反应方程式

HRID 476694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

123 mg of [(RS)-4-methyl-2-[[(S)-3-methyl-1-(methylcarbamoyl)butyl]carbamoyl]-4-methylpentyl](phthalimidomethyl)phosphinic acid methyl ester were dissolved in a mixture of 3 ml of acetic acid and 3 ml of 48% hydrogen bromide in acetic acid and the mixture was left to stand at room temperature for 18 hours. The solvent was removed by evaporation, the residue was dissolved in a mixture of 10 ml of toluene and 5 ml of acetone and the solution was evaporated. This procedure was repeated twice and the residue was then dissolved in a mixture of 5 ml of dichloromethane and 3 ml of acetone and the solution was evaporated. After drying under a high vacuum (0.1 mmHg), there were obtained 115 mg of [(RS)-4-methyl-2-[[(S)-3-methyl-1-(methylcarbamoyl)butyl]carbamoyl]pentyl](phthalimidomethyl)phosphinic acid in the form of an off-white foam.

WORKUP

后处理

  1. waitthe mixture was left
  2. customThe solvent was removed by evaporation
  3. dissolutionthe residue was dissolved in a mixture of 10 ml of toluene and 5 ml of acetone
  4. customthe solution was evaporated
  5. dissolutionthe residue was then dissolved in a mixture of 5 ml of dichloromethane and 3 ml of acetone
  6. customthe solution was evaporated
  7. customAfter drying under a high vacuum (0.1 mmHg)