反应详情

NaH (60%, 6.44 mmol) is added portionwise to a solution of 3-nitro-4-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ylamino)benzonitrile (30, R4=CH3, 4.29 mmol) in DMF (15 mL) at 0° C. The reaction mixture is slowly warmed up to room temperature and stirred for 1 h. To the mixture is added dropwise Mel (6.44 mmol) and the reaction mixture is stirred at room temperature for 5 h. The mixture is diluted with H2O and extracted with Et2O. The organic layer is dried over MgSO4 and evaporated in vacuo. The resulting solid is washed with hexane to give (31) (R4=CH3).

1. additionTo the mixture is added dropwise Mel (6.44 mmol)
2. stirringthe reaction mixture is stirred at room temperature for 5 h
3. extractionextracted with Et2O
4. dry with materialThe organic layer is dried over MgSO4
5. customevaporated in vacuo
6. washThe resulting solid is washed with hexane