HRID1030959
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe resulting mixture is heated at 60° to 80° C.
- temperatureunder reflux for 3 hours
- customAfter removal of residue
- filtrationby filtration
- extractionthe filtrate is extracted with ethyl acetate
- washThe extract is washed with water and sodium bicarbonate solution
- customdried
- concentrationconcentrated