HRID1356663

反应详情

EQUATION

反应方程式

HRID 1356663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4′-Fluoro-2′-nitro-p-toluenesulfonanilide sodium salt (66.46 g (200 mmol)) was dissolved in DMF (66 ml). To this, under heating in an oil bath kept at 120° C., isopropyl iodide (102.0 g (600 mmol)) was added over a period of 20 minutes. The resulting mixture was left to cool to room temperature, mixed with 1% aqueous sodium hydroxide solution and stirred. The resulting crystals were filtered, washed with water and ethanol, successively. The crude crystals thus obtained were recrystallized from ethyl acetate to give 30.58 g (43%) of the title compound as pale yellow crystals.

WORKUP

后处理

  1. temperatureTo this, under heating in an oil bath
  2. customkept at 120° C.
  3. waitThe resulting mixture was left
  4. filtrationThe resulting crystals were filtered
  5. washwashed with water and ethanol
  6. customThe crude crystals thus obtained
  7. customwere recrystallized from ethyl acetate