HRID1030959

反应详情

EQUATION

反应方程式

HRID 1030959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Iron powder (36.42 g) is suspended in 5% aqueous acetic acid (69 ml) and heated to 80° C. To the suspension, a solution of ethyl 5-fluoro-2-nitrophenoxyacetate (15.86 g) in acetic acid (65 ml) and ethyl acetate (65 ml) is dropwise added, and the resulting mixture is heated at 60° to 80° C. under reflux for 3 hours. After removal of residue by filtration, the filtrate is extracted with ethyl acetate. The extract is washed with water and sodium bicarbonate solution, dried and concentrated to give 7-fluoro-3,4-dihydro-3-oxo-2H-1,4-benzoxazine.

WORKUP

后处理

  1. temperaturethe resulting mixture is heated at 60° to 80° C.
  2. temperatureunder reflux for 3 hours
  3. customAfter removal of residue
  4. filtrationby filtration
  5. extractionthe filtrate is extracted with ethyl acetate
  6. washThe extract is washed with water and sodium bicarbonate solution
  7. customdried
  8. concentrationconcentrated