HRID963468

反应详情

EQUATION

反应方程式

HRID 963468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-azatricyclo[4.3.1.14,8 ]undecane (0.30 g) in dichloromethane (4 ml) and water (0.4 ml) was added dropwise a solution of chloroacetyl chloride (0.26 g) in dichloromethane (2 ml) under stirring at cooling in an ice-bath. The mixture was stirred 2 hours under the same condition and then at ambient temperature overnight. The reaction mixture was washed with IN hydrochloric acid aqueous solution and saturated sodium bicarbonate aqueous solution, and dried over sodium sulfate. Removal of the solvent gave N-chloromethylcarbonyl-2-azatricyclo-[4.3.1.14,8 ]undecane (0.33 g), which was used in a following reaction step without further purification.

WORKUP

后处理

  1. temperatureat cooling in an ice-bath
  2. stirringThe mixture was stirred 2 hours under the same condition
  3. customat ambient temperature
  4. customovernight
  5. washThe reaction mixture was washed with IN hydrochloric acid aqueous solution and saturated sodium bicarbonate aqueous solution
  6. dry with materialdried over sodium sulfate
  7. customRemoval of the solvent