反应详情

温度

90 °C

To a solution of 2-chloro-5-methyl-N-[2-(propan-2-ylsulfonyl)phenyl]-pyrimidin-4-amine (0.035 g, 0.11 mmol) in 1 mL of 2-methoxyethanol in a vial was added 4-(dimethylphosphoryl)-2-methyoxyaniline (0.020 g, 0.085 mmol) as the HCl salt. The vial was sealed and the reaction was heated at 90° C. for 16 h. The reaction was quenched with 1N NaOH solution and the solution extracted ethyl acetate. The organic layers were combined, washed with saturated sodium chloride solution, dried with sodium sulfate, filtered and concentrated. The crude residue was purified by silica gel chromatography (0-10% 7N ammonia in methanol:dichloromethane) to afford the desired compound (12 mg, 29% yield). MS/ES+: m/z=489.

1. customThe vial was sealed
2. customThe reaction was quenched with 1N NaOH solution
3. extractionthe solution extracted ethyl acetate
4. washwashed with saturated sodium chloride solution
5. dry with materialdried with sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude residue was purified by silica gel chromatography (0-10% 7N ammonia in methanol:dichloromethane)