HRID333035

反应详情

EQUATION

反应方程式

HRID 333035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The method of Cervena et al.3 was followed. To a stirred solution of 3,4-difluoroaniline (10 mmol) in toluene (5 mL) and pyridine (10 mmol) maintained at 5-10 deg C was added chloroacetyl chloride (10 mmol) in toluene (5 mL) dropwise. The mixture was allowed to stand overnight at room temperature. The organic layer was then separated and the residue was mixed with water (60 mL). The separated solid product was recrystallized from toluene to give N-(3,4-difluorophenyl) chloroacetamide (8.6 g, 84.3% yield). 1HNMR (300 MHz, CDCl3) δ 8.24 (s, 1H, NH), 7.63 (td, J=8.1 Hz, 1H, Ar—H), 7.16-7.12 (m, 2H, Ar—H), 4.19 (s, 2H, COCH2Cl).

WORKUP

后处理

  1. customThe organic layer was then separated
  2. additionthe residue was mixed with water (60 mL)
  3. customThe separated solid product was recrystallized from toluene