HRID464711

反应详情

EQUATION

反应方程式

HRID 464711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

50 g (0.166 moles) of sodium 2-[(2,6-dichlorophenyl)amino]phenylacetate were dissolved in 200 ml of N,N'-dimethylformamide under heating to 50° C., and 41.620 g (0.181 moles) of benzyl bromoacetate were added thereto. Under these conditions stirring was continued for 3 hours. Upon completion of the reaction, the solvent was removed at reduced pressure and the sodium salts were precipitated with addition of 400 ml of ether. The solution was then filtered and the ether phase was washed three times with 100 ml of water and dried on sodium sulphate. The resulting product was concentrated until an oil was obtained, which oil was washed twice with 100 ml of hexane and then crystallized with methanol, thus obtaining 45.28 (61%) of 2-[(2,6-dichlorophenyl)amino]phenylacetoxy acetate.

WORKUP

后处理

  1. customUpon completion of the reaction
  2. customthe solvent was removed at reduced pressure
  3. customthe sodium salts were precipitated with addition of 400 ml of ether
  4. filtrationThe solution was then filtered
  5. washthe ether phase was washed three times with 100 ml of water
  6. customdried on sodium sulphate
  7. concentrationThe resulting product was concentrated until an oil
  8. customwas obtained
  9. washwhich oil was washed twice with 100 ml of hexane
  10. customcrystallized with methanol