反应详情

A mixture of ethyl 3-phenyl-4-(4-chloro-2-aminobenzoyl)-1H-pyrazole-5-carboxylate (0.84 g, 2.28 mmol) and 2-hydroxy-pyridine (0.217 g, 2.28 mmol) in toluene (12 mL) was distilled at 160° C. until all the toluene was removed. The residue was heated at the same temperature for 18 hours. The reaction residue was washed with water to remove the 2-hydroxy-pyridine. The insoluble material was added to methanol (225 mL) and heated to boiling. Ethyl acetate (100 mL) was added and the solution heated for an additional 2 minutes, then concentrated to 100 mL. The solution was filtered to remove some insoluble material and the filtrate concentrated via rotovap until a precipitate formed which was filtered to give the title compound as a tan solid (0.381 g, 51%, mp 328.1-330.9° C.).

1. distillationwas distilled at 160° C. until all the toluene
2. customwas removed
3. temperatureThe residue was heated at the same temperature for 18 hours
4. washThe reaction residue was washed with water
5. customto remove the 2-hydroxy-pyridine
6. additionThe insoluble material was added to methanol (225 mL)
7. temperatureheated to boiling
8. additionEthyl acetate (100 mL) was added
9. temperaturethe solution heated for an additional 2 minutes
10. concentrationconcentrated to 100 mL
11. filtrationThe solution was filtered
12. customto remove some insoluble material
13. concentrationthe filtrate concentrated via rotovap until a precipitate
14. customformed which
15. filtrationwas filtered