HRID1380200
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
A mixture of 1-(3-piperazinylpropyl)-3-n-hexylurea (2.7 g; 10 mmole), 3-trifluoromethyl-4-chlorobenzyl chloride (2.29 g; 10 mmole), triethylamine (1.01 g; 10 mmole) and ethanol (30 ml) was refluxed for 3 hours. The solvent was evaporated in vacuo, and water was added to the residue. The product was extracted with ether, and the extract was dried (sodium sulfate) and concentrated. Precipitation of the oily residue with ethereal hydrochloric acid, followed by recrystallization from alcohol, provided the title compound (3.1 g; 58% yield) as colorless crystals, m.p. 216°-219° C.
WORKUP
后处理
- temperaturewas refluxed for 3 hours
- customThe solvent was evaporated in vacuo, and water
- additionwas added to the residue
- extractionThe product was extracted with ether
- dry with materialthe extract was dried (sodium sulfate)
- concentrationconcentrated
- customPrecipitation of the oily residue with ethereal hydrochloric acid
- customfollowed by recrystallization from alcohol