反应详情

To a solution of 6-(3-amino-2,6-dichloro-phenyl)-2-methylsulfanyl-pyrido[2,3-d]-pyrimidin-7-ylamine (0.5 g, 1.42 mmol) in CH2Cl2 (40 mL) is added 3-(trifluoromethyl)benzoyl chloride (1.07 mL, 7.1 mmol). After the mixture is stirred for 24 hours at room temperature, the mixture is diluted with EtOAc and washed with saturated K2CO3, brine and water. The organic layer is dried, filtered and concentrated to give crude product, which is purified by a flash silica gel column, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH(NH3, 2N)(95/5%), to give the title intermediate as a solid (0.591 g, 79.4 %).

1. washwashed with saturated K2CO3, brine and water
2. customThe organic layer is dried
3. filtrationfiltered
4. concentrationconcentrated
5. customto give crude product, which
6. customis purified by a flash silica gel column
7. washeluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH(NH3, 2N)(95/5%)