HRID661249

反应详情

EQUATION

反应方程式

HRID 661249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.00 g (9.52 mmol, purity 76%) of the compound from Example 76A in dichloromethane (111 ml) was admixed with 4.65 ml (3.37 g, 33.3 mmol) of triethylamine and then, at 0° C., admixed with 1.92 g (9.52 mmol) of 4-nitrophenyl chloroformate. The mixture was warmed to RT and stirred for 2 h. The reaction solution was washed with saturated aqueous sodium hydrogencarbonate solution and water, and the organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. Yield: 5.42 g (94% of theory, purity 80%)

WORKUP

后处理

  1. customat 0° C.
  2. washThe reaction solution was washed with saturated aqueous sodium hydrogencarbonate solution and water
  3. dry with materialthe organic phase was dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure