HRID1579856
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 60.9 g (0.31 mole) of phenacyl bromide in 150 ml. of toluene was added dropwise with stirring to a refluxing solution of 46.6 g. of 1-pyrrolidino-1-cyclohexene in 150 ml. of toluene. The mixture was heated under reflux for 2 hours, diluted with 150 ml. of water, refluxed for 3 hours and cooled. The layers were separated, and the aqueous phase was extracted with ether. The organic solution was dried and concentrated to an oil. Distillation gave 42.1 g. (64%) of orange liquid, b.p. 135°-141° (0.05 mm.), which solidified. Recrystallization from ether-petroleum ether gave tan crystals, m.p. 44°-45°.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 2 hours
- additiondiluted with 150 ml
- temperaturecooled
- customThe layers were separated
- extractionthe aqueous phase was extracted with ether
- customThe organic solution was dried
- concentrationconcentrated to an oil
- distillationDistillation
- customgave 42.1 g
- customRecrystallization from ether-petroleum ether
- customgave tan crystals, m.p. 44°-45°