反应详情

To a solution of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol (60 mg, 0.32 mmol) in DMF (2 mL) was added sodium hydride (55% dispersion in mineral oil, 15 mg, 0.35 mmol). The mixture was stirred at room temperature overnight. After addition of a solution of 6-chloro-1,2,4-triazolo[4,3-b]pyridazine-3-carboxylic acid ethyl ester (79 mg, 0.35 mmol) in DMF (2 mL) the mixture was stirred at room temperature overnight. Then the mixture was evaporated, extracted (ethyl acetate/water) and the organic phase was dried with sodium sulfate and concentrated. Purification by preparative HPLC on reversed phase eluting with acetonitrile/water [0.1% aq NH3 (25%)] afforded the title compound (20 mg, 14%) as a white solid. MS: m/e=380.0 [M+H]+.

1. stirringwas stirred at room temperature overnight
2. customThen the mixture was evaporated
3. extractionextracted (ethyl acetate/water)
4. dry with materialthe organic phase was dried with sodium sulfate
5. concentrationconcentrated
6. customPurification by preparative HPLC on reversed phase
7. washeluting with acetonitrile/water [0.1% aq NH3 (25%)]