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 solution of 1-benzyl-4-piperidone (0.5 g, 2.6 mmol) in THF (10 mL) was cooled to −78° C. and 2-(benzyloxy)phenyl magnesium bromide (3.2 mmol) was added. The mixture was stirred for 0.5 hours then allowed to warm to room temperature. Hydrochloric acid (1 N, 10 mL) was added carefully and the mixture stirred for 0.1 hour before adding a solution of aqueous sodium hydroxide (1 N, 30 mL). The products were extracted into ethyl acetate, dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum. The residue was purified by flash chromatography on silica eluting with 0-50% ethyl acetate/hexane. The fractions containing the desired product were concentrated under vacuum to give the title compound (0.6 g) as a clear, colourless oil.
WORKUP
后处理
- stirringthe mixture stirred for 0.1 hour
- extractionThe products were extracted into ethyl acetate
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customthe solvent removed by evaporation under vacuum
- customThe residue was purified by flash chromatography on silica eluting with 0-50% ethyl acetate/hexane
- additionThe fractions containing the desired product
- concentrationwere concentrated under vacuum