HRID2197435

反应详情

EQUATION

反应方程式

HRID 2197435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.38 ml (3.1 mmol) chloroformic acid ethyl ester were added to 0.8 g (2.8 mmol) of the intermediate product 3b in 20 ml pyridine at 0° C., and then everything was stirred for 16 h at room temperature. Then the batch was poured on to icy water and extracted with ethyl acetate. The organic phase was washed with water, dried and concentrated in a vacuum. The residue obtained in this way was dissolved in a little ether and the product was precipitated by the careful addition of n-pentane. 1.1 g were obtained.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with water
  3. customdried
  4. concentrationconcentrated in a vacuum
  5. customThe residue obtained in this way
  6. customthe product was precipitated by the careful addition of n-pentane
  7. custom1.1 g were obtained