反应详情

A solution of 2-[[3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid (50.2 g, 0.17 mol) in phosphorous oxychloride (120 mL, 1.27 mol) was heated under reflux for 1 hour. The solution was cooled to room temperature and concentrated under reduced pressure, and the residue was poured into iced water. The solution was made basic by the addition of a sodium hydroxide solution, and the organic matter was extracted with chloroform. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (chloroform:methanol=98:2) to give the title compound (21.5 g, 43% yield).

1. temperatureunder reflux for 1 hour
2. concentrationconcentrated under reduced pressure
3. additionthe residue was poured into iced water
4. additionThe solution was made basic by the addition of a sodium hydroxide solution
5. extractionthe organic matter was extracted with chloroform
6. washThe extract was washed with saturated brine and water
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was evaporated under reduced pressure
9. customThe residue thus obtained
10. customwas purified by silica gel column chromatography (chloroform:methanol=98:2)