反应详情

温度

85 °C

A mixture of 4-hydroxy-1,5-dimethyl-6-oxo-1,6-dihydropyridazine-3-carboxylic acid (876 mg, 4.76 mmol) and POCl3 (4.5 mL) was heated for 24 hours at 85° C. POCl3 was removed under reduced pressure. The crude material was quenched with ice. The reaction mixture was stirred for 1 hour at room temperature. After removing solids by filtration, the aqueous filtrate was extracted with EtOAc (3×). The combined organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure to give. The recovered material was combined with the solids previously isolated and triturated with ether to afford 577 mg (60%) of the desired product.

1. customPOCl3 was removed under reduced pressure
2. customThe crude material was quenched with ice
3. customAfter removing solids
4. filtrationby filtration
5. extractionthe aqueous filtrate was extracted with EtOAc (3×)
6. dry with materialThe combined organic layers were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customto give
10. custompreviously isolated
11. customtriturated with ether