反应详情

A solution of 2,6-dichloro-3-nitrophenyl-acetonitrile (1.02 g, 4.42 mmol), 4-amino-pyridine-3-carbaldehyde (0.4 g, 3.28 mmol) and NaOH (52 mg, 1.31 mmol) in EtOH (2.0 mL) is heated to 105° C. for 24 hours. The reaction mixture is diluted with EtOAc (50 ml) and washed with saturated K2CO3 and brine. The organic layer is dried, filtered and concentrated to give crude product. Flash silica gel column purification eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/6) affords the titled intermediate as a solid (257 mg, 23.4%).

1. washwashed with saturated K2CO3 and brine
2. customThe organic layer is dried
3. filtrationfiltered
4. concentrationconcentrated
5. customto give crude product
6. customFlash silica gel column purification
7. washeluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/6)