反应详情

To a solution of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol (76 mg, 0.40 mmol) in DMF (0.8 mL) cooled to 0° C. was added sodium hydride (55% dispersion in mineral oil, 19.2 g, 0.44 mmol). The mixture was stirred at room temperature for 1 h. After addition of 3-chloro-6-(3,5-dimethylpyrazol-1-yl)-pyridazine (91.8 mg, 0.44 mmol) 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. Chromatography (SiO2, heptane:ethanol=100:0 to 95:5) afforded the title compound (5.0 mg, 3%) as a white solid. MS: m/e=362.4 [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