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)-(1-cyano-1,1-diphenylmethyl)piperidine (0.3 g), 2-phenoxyethyl bromide (0.24 g--commercially available), anhydrous potassium carbonate (0.5 g) and acetonitrile (15 ml) was heated under reflux for 5 hours. The mixture was then partitioned between dichloromethane (30 ml) and 10% aqueous potassium carbonate (30 ml), the layers separated, and the aqueous layer extracted with dichloromethane (2×20 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 2%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a gum, yield 0.254 g.
WORKUP
后处理
- temperatureunder reflux for 5 hours
- customThe mixture was then partitioned between dichloromethane (30 ml) and 10% aqueous potassium carbonate (30 ml)
- customthe layers separated
- extractionthe aqueous layer extracted with dichloromethane (2×20 ml)
- dry with materialThe combined dichloromethane extracts were dried (MgSO4)
- concentrationconcentrated in vacuo
- customto give a gum which
- customwas purified by column chromatography on silica eluting with dichloromethane
- additioncontaining methanol (0% up to 2%)
- concentrationconcentrated in vacuo