HRID583063
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
Powdered potassium hydroxide (144.4 g) was added carefully to a mechanically stirred mixture of 6-fluoroindole (49.23 g, 0.364 mol) and 4-piperidone monohydrate (111.93 g, 0.728 mol) in methanol (1500 ml). The mixture was then heated under reflux under nitrogen for 18 hours and then more potassium hydroxide (40 g) was added and the reaction mixture heated under reflux for a further 4 hours. The reaction mixture was allowed to cool to room temperature and poured onto ice-water (3000 ml) and stirred for 1 hour and the precipitated solid isolated by filtration and dried at 50° C. in vacuo to give a solid.
WORKUP
后处理
- temperatureThe mixture was then heated
- temperatureunder reflux under nitrogen for 18 hours
- temperaturethe reaction mixture heated
- temperatureunder reflux for a further 4 hours
- additionpoured onto ice-water (3000 ml)
- customthe precipitated solid isolated by filtration
- customdried at 50° C. in vacuo
- customto give a solid