HRID1248273

反应详情

EQUATION

反应方程式

HRID 1248273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.00 gram (4.22 mmoles) of the 2-azido-3-phenylmercapto-propionic acid methyl ester obtained in Example 2 was dissolved in 5 ml of acetic anhydride and then was added 1 mole % of rhenium VII sulfide based on the azido compound employed. Under vigorous stirring there was led hydrogen through the solution for 24 hours at 70° C. After the end of the reaction the solvent was drawn off under reduced pressure on the rotary evaporator, the product taken up in diethyl ether and the catalyst filtered off. Chromatography on a silica gel column with petroleum ether/ethyl acetate (volume ratio 1:1) gave 0.50 gram (47% of theory) of N-acetyl-S-phenyl-cysteine methyl ester as a colorless oil.

WORKUP

后处理

  1. customfor 24 hours
  2. customat 70° C
  3. customAfter the end of the reaction the solvent
  4. customwas drawn off under reduced pressure on the rotary evaporator
  5. filtrationthe catalyst filtered off