HRID464244
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
7 Grams (0.0188 mole) of the compound prepared under (A) were dissolved in 80 ml of anhydrous benzene, and the resulting solution was added with 8 ml (0.0574 mole) of triethylamine and 5 g (0.0281 mole) of nicotinoylchloride suspended in 20 ml of anhydrous benzene. The reaction mixture was heated for 24 hours on an oil bath at 55°-60° C. under stirring then, after cooling, it was twice washed with water and the organic phase was dried over sodium sulfate. The organic solvent was removed in vacuo until formation of a precipitate then, after complete precipitation, the obtained solid was recovered by filtration, washed with anhydrous diethyl ether and dried overnight at 70° C.
WORKUP
后处理
- temperatureThe reaction mixture was heated for 24 hours on an oil bath at 55°-60° C.
- temperatureafter cooling
- washit was twice washed with water
- dry with materialthe organic phase was dried over sodium sulfate
- customThe organic solvent was removed in vacuo until formation of a precipitate
- customafter complete precipitation
- filtrationthe obtained solid was recovered by filtration
- washwashed with anhydrous diethyl ether
- customdried overnight at 70° C.