反应详情

To a solution of 3-chloro-6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazine (200 mg, 0.66 mmol) in a mixture of methanol (3 mL) and THF (1 mL) was added dropwise sodium methoxide (5.4 M in MeOH, 0.16 mL, 0.86 mmol) and the reaction mixture was heated under reflux for 24 h. After dilution with tert-butylmethylether (4 mL) and water (2 mL) it was extracted with tert-butylmethylether (15 mL) and dried over sodium sulfate. Concentration and purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 50:50) afforded the title compound (56 mg, 27%) as a colorless oil. MS: m/e=298.3 [M+H]+.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 24 h
3. extractionAfter dilution with tert-butylmethylether (4 mL) and water (2 mL) it was extracted with tert-butylmethylether (15 mL)
4. dry with materialdried over sodium sulfate
5. concentrationConcentration and purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 50:50)