反应详情

135.8 g (0.67 mol) of methyl-(2-nitrobenzyl)-amine and 187.5 ml (1.339 mols) of triethylamine are dissolved in 1.87 liters of ethanol at room temperature, with stirring, and 148 g (0.682 mol) of 2-bromo-1-(4-fluorophenyl)ethanone are then added in portions. The reaction mixture is stirred for 3 hours. The solvent is then stripped off on a rotary evaporator and the residue is dissolved in 1.3 liters of toluene. The toluene phase is washed several times with H2O and dried over Na2SO4, and HCl/diethyl ether is added. The glutinous precipitate is separated from the toluene by decanting and crystallized with acetone. The colorless precipitate is filtered off with suction and dried.

1. stirringThe reaction mixture is stirred for 3 hours
2. customThe solvent is then stripped off on a rotary evaporator
3. dissolutionthe residue is dissolved in 1.3 liters of toluene
4. washThe toluene phase is washed several times with H2O
5. dry with materialdried over Na2SO4, and HCl/diethyl ether
6. additionis added
7. customThe glutinous precipitate is separated from the toluene
8. customby decanting
9. customcrystallized with acetone
10. filtrationThe colorless precipitate is filtered off with suction
11. customdried