HRID2399608

反应详情

EQUATION

反应方程式

HRID 2399608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To 52.1 g of N-(5-nitro-2-phenoxyphenyl)methanesulfonamide was added 51 ml of an aqueous solution containing 2.7 g of ammonium chloride, and then 42.5 g of an iron powder was added thereto with heating at 80° C. with stirring, followed by stirring for 2 hours. To the reaction cooled to 50° C. were added ethyl acetate and water, and the precipitate was filtered. After extraction with ethyl acetate, the organic layer was successively washed with water and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was recrystallized from ethanol to give 29.6 g of N-(5-amino-2-phenoxyphenyl)methanesulfonamide.

WORKUP

后处理

  1. stirringby stirring for 2 hours
  2. temperatureTo the reaction cooled to 50° C.
  3. filtrationthe precipitate was filtered
  4. extractionAfter extraction with ethyl acetate
  5. washthe organic layer was successively washed with water
  6. dry with materiala saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated
  8. customthe residue was recrystallized from ethanol