HRID2073482

反应详情

EQUATION

反应方程式

HRID 2073482 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

31.1 g (0.100 mol) of 3,3-bis(4-fluorophenyl)propyl bromide, 20.6 g (0.130 mol) of ethyl piperazine-1-carboxylate, 27.6 g (0.200 mol) of powdered potassium carbonate and 4.15 g of potassium iodide were heated at the reflux temperature in 400 ml of toluene for 31 hours; the precipitate was then filtered off and the filtrate was concentrated. The material thus obtained was dissolved in 450 ml of ethanol, 450 ml of 4N KOH were added and the mixture was heated under reflux for 9 hours. After customary working up (compare Example 3d), 26.8 g of product, melting point 58°-64° C., were obtained.

WORKUP

后处理

  1. filtrationthe precipitate was then filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe material thus obtained
  4. temperaturethe mixture was heated
  5. temperatureunder reflux for 9 hours