HRID275394
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 8.6 of 1-(2-chloroethyl)-1-ethyl-3,4-dihydro-6,7-dimethoxy-1H-2-benzopyran, 8 g of 1-[3,3-bis(4-fluorophenyl)propyl]piperazine, 5.2 g of potassium carbonate and 0.4 g of potassium iodide in 100 ml of dimethylformamide was refluxed for 4 h. Water was added and the base was extracted twice with ethyl acetate. After washing, drying and evaporation the difumarate was prepared in absolute ethanol to yield 13.2 g (61.2%) of 1-[2-(1-ethyl-3,4-dihydro-6,7-dimethoxy-1H-2-benzopyran-1-yl)ethyl]-4-[3,3-bis (4-fluorophenyl)propyl]piperazine (E)-2-butenedioate (1:2) salt.
WORKUP
后处理
- temperaturewas refluxed for 4 h
- extractionthe base was extracted twice with ethyl acetate
- washAfter washing
- customdrying
- customevaporation the difumarate
- customwas prepared in absolute ethanol