HRID1789893

反应详情

EQUATION

反应方程式

HRID 1789893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of KOH (0.26 g; 4.6 mmol) in ethanol (7 mL) was added to a solution of 2-(1-tert-butoxycarbonyl-pyrrolidin-3-ylmethyl)-malonic acid diethyl ester (1.52 g; 4.4 mmol) in ethanol (7 mL) at 0° C. The reaction mixture was stirred at room temperature overnight, concentrated under reduced pressure and the residue was dissolved in water (500 mL). The aqueous layer was washed with diethyl ether, acidified to pH. 3 by 0.5 M HCl, and extracted with diethyl ether. The organic phase was dried and concentrated under reduced pressure to yield 2-(1-tert-butoxycarbonyl-pyrrolidin-3-ylmethyl)-malonic acid monoethyl ester (1.13 g, 81%).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionthe residue was dissolved in water (500 mL)
  3. washThe aqueous layer was washed with diethyl ether
  4. extraction3 by 0.5 M HCl, and extracted with diethyl ether
  5. customThe organic phase was dried
  6. concentrationconcentrated under reduced pressure