反应详情

A solution of 4-chloro-2,6-dimethyl-3-nitropyridine (9.80 g, 52.5 mmol) and 4-aminobenzonitrile (6.20 g, 52.5 mmol) in ethanol (160 ml) was stirred at room temperature for 16 hours. The solvent was removed under reduced pressure and the residue was dissolved in dichloromethane (200 ml), and washed with saturated aqueous sodium bicarbonate (100 ml). The organic phase was dried (MgSO4) and concentrated under reduced pressure to give a gum which was crystallised by adding ether (100 ml) and sonicating for 5 minutes. The yellow solid (9.80 g, 70%) was filtered off and dried in vacuo, mp 171°-172° C.

1. customThe solvent was removed under reduced pressure
2. dissolutionthe residue was dissolved in dichloromethane (200 ml)
3. washwashed with saturated aqueous sodium bicarbonate (100 ml)
4. dry with materialThe organic phase was dried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customto give a gum which
7. customwas crystallised
8. additionby adding ether (100 ml)
9. customsonicating for 5 minutes
10. filtrationThe yellow solid (9.80 g, 70%) was filtered off
11. customdried in vacuo, mp 171°-172° C.