HRID1388228

反应详情

EQUATION

反应方程式

HRID 1388228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

20 g of 2-amino-4-chloro-5-nitrophenol was dispersed in 150 ml of acetonitrile to which 37.7 g of 2-(2,4-di-tert-amylphenoxy)butanoyl chloride was added dropwise under refluxing. After refluxing for 4 hours, the reaction mixture was cooled to deposit crystals. The crystals were collected by filtration, washed with acetonitrile and dried to yield 49.5 g thereof. 49 g of the crystals were refluxed with stirring for 1 hour together with 28 g of reduced iron powder, 2.7 g of ammonium chloride, 50 ml of water and 500 ml of isopropanol. After removing the iron powder by filtration, the filtrate was cooled to deposite the crystals. The crystals were collected by filtration and dried to obtain 42.4 g of the above described compound.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureunder refluxing
  3. temperatureAfter refluxing for 4 hours
  4. temperaturethe reaction mixture was cooled
  5. filtrationThe crystals were collected by filtration
  6. washwashed with acetonitrile
  7. customdried
  8. customto yield 49.5 g
  9. customAfter removing the iron powder
  10. filtrationby filtration
  11. temperaturethe filtrate was cooled
  12. filtrationThe crystals were collected by filtration
  13. customdried
  14. customto obtain 42.4 g of the