反应详情

Step 1): A solution of bromodiphenylmethane (48.2 g, 195 mmol) in DMSO (30 ml) was added dropwise to a solution of nipecotamide (25 g, 195 mmol) and K2CO3 (27 g, 195 mmol) in CH3CN (100 ml) and DMSO (50 ml) under stirring and cooling in an ice-bath for 1 hour. After the addition was complete, the mixture was stirred overnight at room temperature. The insoluble precipitates were filtered off and then the filtrate was evaporated. To the residue was added H2O and AcOEt, and agitated. The organic layer was washed with H2O, dried over MgSO4 and evaporated to give 1-diphenylmethylpiperidin-3-carboxamide, 33 g (57.5%): mp 86°-87° C.

1. temperaturecooling in an ice-bath for 1 hour
2. additionAfter the addition
3. stirringthe mixture was stirred overnight at room temperature
4. customThe insoluble precipitates
5. filtrationwere filtered off
6. customthe filtrate was evaporated
7. additionTo the residue was added H2O and AcOEt
8. stirringagitated
9. washThe organic layer was washed with H2O
10. dry with materialdried over MgSO4
11. customevaporated