HRID2073482
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
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
- filtrationthe precipitate was then filtered off
- concentrationthe filtrate was concentrated
- customThe material thus obtained
- temperaturethe mixture was heated
- temperatureunder reflux for 9 hours