HRID1402840

反应详情

EQUATION

反应方程式

HRID 1402840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The solution of ethyl 3-(4-chlorophenyl)-4-nitrobutanoate (2.33 g) in acetic acid (18 ml) was stirred vigorously while iron powder (5.7 g) was added. The suspension was stirred at reflux temperature for 1.5 h. The resulting thick slurry was pored into a mixture of conc. HCl (30 ml) and ice (30 g). The aqueous layer was extracted with dichloromethane (2×50 ml) and the combined organic layers washed with water and dried (sodium sulfate). After evaporation of the solvent the oily residue was distilled with toluene to remove acetic acid whereupon crystallisation took place. The crude was washed with diethyl ether (3×2 ml) and dried in vacuo to afford 4-(4-chlorophenyl)-2-pyrrolidone (0.86 g) as colourless crystals.

WORKUP

后处理

  1. additionwas added
  2. temperatureat reflux temperature for 1.5 h
  3. extractionThe aqueous layer was extracted with dichloromethane (2×50 ml)
  4. washthe combined organic layers washed with water
  5. dry with materialdried (sodium sulfate)
  6. customAfter evaporation of the solvent the oily residue
  7. distillationwas distilled with toluene
  8. customto remove acetic acid
  9. customwhereupon crystallisation
  10. washThe crude was washed with diethyl ether (3×2 ml)
  11. customdried in vacuo