HRID275394

反应详情

EQUATION

反应方程式

HRID 275394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas refluxed for 4 h
  2. extractionthe base was extracted twice with ethyl acetate
  3. washAfter washing
  4. customdrying
  5. customevaporation the difumarate
  6. customwas prepared in absolute ethanol