反应详情

To a solution of N-[3-(7-amino-2-methylsulfanyl-pyrido[2,3-d]pyrimidin-6-yl)-2,4-dichloro-phenyl]-3-trifluoromethyl-benzamide (1.7 g, 3.24 mmol) in TFA (15 mL) is slowly added NaNO2 (783 mg, 11.35 mmol) at 0° C. with stirring for 20 minutes. The solvents are evaporated and diluted with EtOAc and washed with saturated K2CO3, brine and water. The organic layer is dried, filtered and concentrated to give the crude product. The crude product is purified by flash silica gel column, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH(NH3, 2N)(93/7%), to give the title intermediate as a solid (1.64 g, 96.5%).

1. customat 0° C.
2. customThe solvents are evaporated
3. additiondiluted with EtOAc
4. washwashed with saturated K2CO3, brine and water
5. customThe organic layer is dried
6. filtrationfiltered
7. concentrationconcentrated
8. customto give the crude product
9. customThe crude product is purified by flash silica gel column
10. washeluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH(NH3, 2N)(93/7%)