HRID1253011

反应详情

EQUATION

反应方程式

HRID 1253011 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, and 37.7 g of 2-(2,4-di-t-amylphenoxy)butanoyl chloride was added thereto dropwise under refluxing. After stirring while refluxing for 1 hour, the reaction mixture was cooled to room temperature, and the crystals thus formed were collected by filtration, washed with acetonitrile, and dried to obtain crystals weighing 49.5 g. A mixture of 49 g of the resulting crystals, 28 g of reduced iron, 2.7 g of ammonium chloride, 50 ml of water, and 500 ml of isopropanol was stirred while refluxing for 1 hour. The iron powder was removed by filtration, and the filtrate was cooled to precipitate crystals, which were then collected by filtration and dried to provide 42.4 g of the desired compound.

WORKUP

后处理

  1. temperaturedropwise under refluxing
  2. temperaturewhile refluxing for 1 hour
  3. customthe crystals thus formed
  4. filtrationwere collected by filtration
  5. washwashed with acetonitrile
  6. customdried
  7. customto obtain crystals
  8. stirringwas stirred
  9. temperaturewhile refluxing for 1 hour
  10. customThe iron powder was removed by filtration
  11. temperaturethe filtrate was cooled
  12. customto precipitate crystals, which
  13. filtrationwere then collected by filtration
  14. customdried