HRID75183

反应详情

EQUATION

反应方程式

HRID 75183 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 3-chloro-N-hydroxy-2-oxopropanimidoyl chloride (0.89 g, 5.71 mmol) in acetonitrile (20 mL) was added 2-ethenyl-1,3-difluorobenzene (1.0 g, 7.14 mmol) and sodium bicarbonate (1.8 g, 2.14 mmol) at room temperature. The reaction mixture was stirred at room temperature for 12 h, concentrated in under reduced pressure and the resulting material was partitioned between ethyl acetate (50 mL) and water (50 mL). The organic layer was separated, washed with saturated aqueous sodium chloride solution and concentrated in under reduced pressure. The resulting material was triturated with petroleum ether and filtered to provide the title product as white solid (1.1 g) melting at 82.1-83.4° C.

WORKUP

后处理

  1. concentrationconcentrated in under reduced pressure
  2. customthe resulting material was partitioned between ethyl acetate (50 mL) and water (50 mL)
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous sodium chloride solution
  5. concentrationconcentrated in under reduced pressure
  6. customThe resulting material was triturated with petroleum ether
  7. filtrationfiltered