HRID565721

反应详情

EQUATION

反应方程式

HRID 565721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl (RS)-2,5-dibromovalerate (24.5 g) and toluene (19.8 g) were added to a 49% aqueous potassium carbonate solution (53.3 g), and heated to 80° C. (S)-α-methylbenzylamine (12.0 g) was added dropwise to the mixture obtained above at that temperature, and was stirred at that temperature for 9.5 hours. Water (33.9 g) was added to the reaction mixture, and then the organic layer was separated from the resulting mixture. Separated organic layer was washed with water, a 1% aqueous hydrochloric acid solution and water in this order, and concentrated under reduced pressure. Thus, N-[(S)-α-methylbenzyl]-(RS)-proline methyl ester (16.3 g) was obtained in a yield of 77.8%.

WORKUP

后处理

  1. additionwas added dropwise to the mixture
  2. customobtained above at that temperature
  3. customthe organic layer was separated from the resulting mixture
  4. washSeparated organic layer was washed with water
  5. concentrationa 1% aqueous hydrochloric acid solution and water in this order, and concentrated under reduced pressure