HRID729078
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
2,8-Dimethyl-3-(2-chloroethyl)-4-chloroquinoline (7.63 g, 30 mmol) and 2-methylaniline hydrochloride (4.31 g, 30 mmol) in 1-butanol (100 ml) wereheated at reflux for 4 days, then the solvent evaporated, the crude producttaken up in dichloromethane, washed with aqueous sodium bicarbonate, dried and evaporated. Chromatography (silica gel, 2% methanolic ammonia in dichloromethane) and recrystallisation from aqueous ethanol gave 1-(2-methylphenyl)-4,6-dimethyl-2,3-dihydropyrrolo-[3,2-c]quinoline (1.95 g, 23%), m.p. 126°-128°.
WORKUP
后处理
- temperatureat reflux for 4 days
- customthe solvent evaporated
- washwashed with aqueous sodium bicarbonate
- customdried
- customevaporated
- customChromatography (silica gel, 2% methanolic ammonia in dichloromethane) and recrystallisation from aqueous ethanol