反应详情

温度

110 °C

A mixture of 4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (2.0 g, 11.82 mmol), (3-amino-2,6-dichloro-phenyl)-acetonitrile (2.85 g, 14.18 mmol) and K2CO3 (4.9 g, 35.49 mmol) in DMF (20 mL) is heated to 110° C. for 30 hours. The solution is cooled to room temperature and the solid is removed by filter paper and concentrated to give crude product. Flash silica gel column purification, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%), gives the title intermediate as a solid (3.31 g, 80.0%).

1. temperatureThe solution is cooled to room temperature
2. customthe solid is removed
3. filtrationby filter paper
4. concentrationconcentrated
5. customto give crude product
6. customFlash silica gel column purification
7. washeluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%)