HRID1580625
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe precipitate was filtered
- washwashed with water
- additionThe precipitate was added to 180 ml of 5 % ethanolic hydrogen chloride
- temperaturethe mixture was heated
- temperatureunder reflux for 4 hours
- distillationThe solvent was distilled off under reduced pressure to the residue, to which
- additionwas added 100 ml of water
- customThe resulting solid substance was recrystallized from ethanol