HRID21397
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 containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)piperidine (0.3 g), phenethyl bromide (0.2 g), anhydrous potassium carbonate (0.3 g) and acetonitrile (10 ml) was heated under reflux for 7 hours. The mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml), the layers separated, and the aqueous layer extracted with dichloromethane (2×30 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a colourless solid which was recrystallised from aqueous ethanol to give the title compound, yield, 0.17 g, m.p. 175°-1780° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 7 hours
- customThe mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml)
- customthe layers separated
- extractionthe aqueous layer extracted with dichloromethane (2×30 ml)
- dry with materialThe combined dichloromethane extracts were dried (MgSO4)
- concentrationconcentrated in vacuo
- customto give a colourless solid which
- customwas recrystallised from aqueous ethanol