反应详情

A mixture of the crude 3-(2-chlorophenyl)-6-(2,4-difluorophenoxy)-4-methyl-5-oxo-4,5-dihydro-pyrazolo[4,3-b]pyridine-1-carboxylic acid tert-butyl ester (0.0298 mmol) in a solution of 0.5 M sodium methoxide in methanol (Aldrich) (7 mL) was stirred at room temperature for 1 hour. The solvent was removed under reduced pressure at 55° C., and the resulting residue was diluted with ethyl acetate (35 mL) and water (25 mL). The organic layer was separated, washed with brine (1×25 mL), dried over magnesium sulfate, filtered, concentrated, and purified by Preparative Thin Layer Chromatography eluting with 60% ethyl acetate in hexanes to give the title compound (5.2 mg, (M+H)+=388) as a white powder.

1. customThe solvent was removed under reduced pressure at 55° C.
2. additionthe resulting residue was diluted with ethyl acetate (35 mL) and water (25 mL)
3. customThe organic layer was separated
4. washwashed with brine (1×25 mL)
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by Preparative Thin Layer Chromatography
9. washeluting with 60% ethyl acetate in hexanes