HRID1656441
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
A mixture of 2-amino-2'-chloro-3,5-dimethylbenzophenone (20.0 g), 2,2-dimethoxypropionitrile (11.5 g), p-toluenesulfonic acid hydrate (1.46 g) and toluene (200 ml) was refluxed for 3 hrs., with removal of water by a Dean-Stark apparatus. The mixture was washed with sodium hydrogen carbonate solution and water, dried over anhydrous magnesium sulfate and distilled to remove the solvent. The resultant precipitate was collected by filtration and washed with hexane to give 4-(2-chlorophenyl)-6,8-dimethyl-3-quinolinecarbonitrile (20.7 g, 92.0%), which was recrystallized from ethanol to give pale yellow plates. m.p. 153°-154° C.
WORKUP
后处理
- temperaturewas refluxed for 3 hrs
- custom, with removal of water by a Dean-Stark apparatus
- washThe mixture was washed with sodium hydrogen carbonate solution and water
- dry with materialdried over anhydrous magnesium sulfate
- distillationdistilled
- customto remove the solvent
- filtrationThe resultant precipitate was collected by filtration
- washwashed with hexane