反应详情

温度

107.5 °C

A mixture of 1.62 g of 4-chloro-1-(4-methoxy-phenyl)-butan-1-one (1), 1.20 g of 4-(4-methyl-benzyl)-piperidin-4-ol (2), 1.62 g of K2CO3, and 0.49 g of KI in acetonitrile (30 mL) was stirred and refluxed at 105 to 110° C. for 9 hours under nitrogen atmosphere. After the solvent was removed, ice water was added and the mixture was extracted with ethyl acetate. The organic layer was successively washed with water and brine and dried over MgSO4. After the solvent was removed, the obtained oily residue was purified by silica gel chromatography (chloroform:methanol=20/1 to 10/1) and the purified product was recrystallized from AcOEt/Et2O to afford 1.73 g of compound (3).

1. customAfter the solvent was removed
2. additionice water was added
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was successively washed with water and brine
5. dry with materialdried over MgSO4
6. customAfter the solvent was removed
7. customthe obtained oily residue was purified by silica gel chromatography (chloroform:methanol=20/1 to 10/1)
8. customthe purified product was recrystallized from AcOEt/Et2O