HRID880508
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 1-(4-fluoro-5-nitro-indolin-1-yl)ethanone (0.56 g, 2.51 mmol) and concentrated hydrochloric acid (10 mL) was refluxed for 16 h. The reaction mixture was cooled to ambient temperature and partitioned between chlorofolin (100 mL) and water (100 mL). The organic layer was separated and the aqueous layer extracted with chloroform (5×30 mL). The combined organic layers were washed with water (3×20 mL), brine (3×20 mL) and dried over anhydrous sodium sulphate. Concentration in vacuo afforded 4-fluoro-5-nitro-indoline (0.35 g, 76%) as a yellow solid.
WORKUP
后处理
- temperaturewas refluxed for 16 h
- custompartitioned between chlorofolin (100 mL) and water (100 mL)
- customThe organic layer was separated
- extractionthe aqueous layer extracted with chloroform (5×30 mL)
- washThe combined organic layers were washed with water (3×20 mL), brine (3×20 mL)
- dry with materialdried over anhydrous sodium sulphate
- concentrationConcentration in vacuo