HRID35298

反应详情

EQUATION

反应方程式

HRID 35298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 21.9 parts of 4-fluoro-α-(4-fluorophenyl)benzenemethanamine in 160 parts of 2-propanone were added 11.66 parts of sodium carbonate. Then there were added dropwise 12.43 parts of 2-chloroacetyl chloride at a temperature below 30° C. (cooling in an ice-bath was necessary). Upon completion, stirring was continued first for one hour at room temperature and further for 2 hours at reflux. After cooling to room temperature, the sodium carbonate was filtered off and washed with 2-propanone. The filtrate was evaporated and the residue was crystallized from 2,2'-oxybispropane, yielding 20.6 parts of N-[bis(4-fluorophenyl)-methyl]-2-chloroacetamide; mp. 127.6° C. (intermediate 4).

WORKUP

后处理

  1. temperatureat a temperature below 30° C. (cooling in an ice-bath was necessary)
  2. temperatureat reflux
  3. filtrationthe sodium carbonate was filtered off
  4. washwashed with 2-propanone
  5. customThe filtrate was evaporated
  6. customthe residue was crystallized from 2,2'-oxybispropane