HRID2166077

反应详情

EQUATION

反应方程式

HRID 2166077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product of stage (ii) (0.080 g) in dry acetonitrile (10 ml) was treated with a solution of methyl chloroformate (71 mg; 0.75 mmol) in dry acetonitrile (3 ml) over a 5 min period. The mixture was stirred at ambient temperature for 30 min and aqueous sodium carbonate solution (1 ml) was added. The solvent was removed in vacuo and the aqueous residue was extracted with dichloromethane (3×25 ml) and chloroform (3×25 ml). The extract was washed with aqueous sodium carbonate solution (5 ml: 1M), and the combined extracts were dried and evaporated in vacuo to give the title compound as an oil (0.1 g).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. extractionthe aqueous residue was extracted with dichloromethane (3×25 ml) and chloroform (3×25 ml)
  3. washThe extract was washed with aqueous sodium carbonate solution (5 ml: 1M)
  4. customthe combined extracts were dried
  5. customevaporated in vacuo