反应详情

温度

180 °C

To 89 mg of 6-chloro-4-[(3,5-difluorobenzyl)amino]pyridine-3-carboxyamide (the compound of Example 20) suspended in 3 mL of diphenylether, 65 mg of 1,2-phenylenediamine and 144 mg of methanesulfonic acid were added, and stirred in a nitrogen atmosphere at 180° C. for 30 minutes. After cooling, chloroform was added to the reaction mixture to dissolve the deposit, washed with saturated sodium bicarbonate, and dried on anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (chloroform:methanol:ammonia water=10:1:0.1) to obtain 18 mg (yield 17%) of the title compound as a light brown powder.

1. temperatureAfter cooling
2. dissolutionto dissolve the deposit
3. washwashed with saturated sodium bicarbonate
4. dry with materialdried on anhydrous sodium sulfate
5. customThe solvent was evaporated
6. customthe residue was purified by silica gel column chromatography (chloroform:methanol:ammonia water=10:1:0.1)