HRID1580625

反应详情

EQUATION

反应方程式

HRID 1580625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 10.8 g of phenylhydrazine in 100 ml of 30 % aqueous acetic acid was added 27.4 g of 1-(γ-acetylbutyryl)-4-phenylpiperazine and the resulting mixture was stirred for 30 minutes at room temperature. The precipitate was filtered, and washed with water. The precipitate was added to 180 ml of 5 % ethanolic hydrogen chloride, and the mixture was heated under reflux for 4 hours. The solvent was distilled off under reduced pressure to the residue, to which was added 100 ml of water. The resulting solid substance was recrystallized from ethanol to give 1-[β-(2-methyl-3-indolyl)propionyl]-4-phenylpiperazine, melting at 120°-121°C.

WORKUP

后处理

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. additionThe precipitate was added to 180 ml of 5 % ethanolic hydrogen chloride
  4. temperaturethe mixture was heated
  5. temperatureunder reflux for 4 hours
  6. distillationThe solvent was distilled off under reduced pressure to the residue, to which
  7. additionwas added 100 ml of water
  8. customThe resulting solid substance was recrystallized from ethanol