HRID2238526

反应详情

EQUATION

反应方程式

HRID 2238526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Methyl 1-cyclopentyl-5-oxoprolinate (0.560 g, 2.65 mmol) was dissolved in ethanol (10 ml) and cooled to 0° C. in an ice-bath. 2M aqueous sodium hydroxide (5 ml) was added and the mixture was stirred at ice temperature for 4 hrs. The ethanol was then evaporated under vacuum and the aqueous residue was acidified to pH1 by the addition of 2N aqueous hydrogen chloride. The volume of resulting aqueous mixture was reduced under vacuum to ˜3 ml and this was then extracted with a 3:1 mixture of chloroform and isopropanol respectively using a phase separator. The aqueous layer was washed with more dichloromethane and then the combined organic fractions were evaporated to give crude 1-cyclopentyl-5-oxoproline which was used in subsequent reactions without further purification.

WORKUP

后处理

  1. customThe ethanol was then evaporated under vacuum
  2. additionthe aqueous residue was acidified to pH1 by the addition of 2N aqueous hydrogen chloride
  3. extractionthis was then extracted with a 3:1 mixture of chloroform and isopropanol
  4. washThe aqueous layer was washed with more dichloromethane
  5. customthe combined organic fractions were evaporated