HRID1389939

反应详情

EQUATION

反应方程式

HRID 1389939 的结构方程式

PROCEDURE

实验过程

A mixture of 12.7 parts of 2-(2,6-dichlorophenyl)-2-(2-naphthylamino) acetamide and 250 parts of potassium hydroxide/ethanol 1 N is stirred and refluxed for 48 hours. The reaction mixture is evaporated. The oily residue is dissolved in 400 parts of water and the solution is acidified with concentrated hydrochloric acid solution. The sticky product is extracted with 1,1'-oxybisethane. The extract is washed twice with water, dried and evaporated. The oily residue is triturated three times in petroleumether. The solid product is filtered off and recrystallized from 50 parts of glacial acetic acid. The product is washed with petroleumether, dried and dissolved in 80 parts of 1,1'-oxybisethane. The solution is stirred with activated charcoal, filtered and the filtrate is evaporated. The oily residue solidifies on triturating in 2-propanol and petroleumether. The solid is filtered off and dried, yielding 1.6 parts of 2-(2,6-dichlorophenyl)-N-(2-naphthyl)glycine; mp. 171.7° C.

WORKUP

后处理

  1. temperaturerefluxed for 48 hours
  2. customThe reaction mixture is evaporated
  3. dissolutionThe oily residue is dissolved in 400 parts of water
  4. extractionThe sticky product is extracted with 1,1'-oxybisethane
  5. washThe extract is washed twice with water
  6. customdried
  7. customevaporated
  8. customThe oily residue is triturated three times in petroleumether
  9. filtrationThe solid product is filtered off
  10. customrecrystallized from 50 parts of glacial acetic acid
  11. washThe product is washed with petroleumether
  12. customdried
  13. dissolutiondissolved in 80 parts of 1,1'-oxybisethane
  14. stirringThe solution is stirred with activated charcoal
  15. filtrationfiltered
  16. customthe filtrate is evaporated
  17. customon triturating in 2-propanol
  18. filtrationThe solid is filtered off
  19. customdried