HRID880508

反应详情

EQUATION

反应方程式

HRID 880508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas refluxed for 16 h
  2. custompartitioned between chlorofolin (100 mL) and water (100 mL)
  3. customThe organic layer was separated
  4. extractionthe aqueous layer extracted with chloroform (5×30 mL)
  5. washThe combined organic layers were washed with water (3×20 mL), brine (3×20 mL)
  6. dry with materialdried over anhydrous sodium sulphate
  7. concentrationConcentration in vacuo