HRID923784

反应详情

EQUATION

反应方程式

HRID 923784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture of (2,6-dinitro-4-trifluoromethyl-phenyl)-methyl-amine (5.0 g), acetic acid (11 mL), ethanol (100 ml), and ice (20 g), iron powder (6.4 g) was added under ice-cooling. The reaction mixture was stirred at 0° C. for 3.5 hours, and filtered through Celite®. The resulting filtrate was concentrated under reduced pressure, and diluted with 1N aqueous sodium hydroxide solution. The solution was extracted with ethyl acetate. The combined organic layer was dried over sodium sulfate, and concentrated under reduced pressure to give 3.1 g of N′-methyl-5-trifluoromethyl-benzene-1,2,3-triamine. N′-methyl-5-trifluoromethyl-benzene-1,2,3-triamine

WORKUP

后处理

  1. additionwas added under ice-
  2. temperaturecooling
  3. filtrationfiltered through Celite®
  4. concentrationThe resulting filtrate was concentrated under reduced pressure
  5. additiondiluted with 1N aqueous sodium hydroxide solution
  6. extractionThe solution was extracted with ethyl acetate
  7. dry with materialThe combined organic layer was dried over sodium sulfate
  8. concentrationconcentrated under reduced pressure