反应详情

To a solution of aminomethylcyclopropane (0.11 mL, 1.2 mmol) in dioxane (5 mL) was added dropwise trimethylaluminum solution (2 M solution in hexane, 0.62 mL, 1.24 mmol). After stirring for 1 h at room temperature a suspension of 6-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyridazine-3-carboxylic acid methyl ester (100 mg, 0.3 mmol) in dioxane (5 mL) was added. The reaction mixture was stirred at 90° C. for 2 h, cooled to room temperature and poured into water. Extraction (ethyl acetate/saturated aqueous Seignette salt solution) followed by drying of the organic phase over sodium sulfate and evaporation afforded an oil. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 0:100) afforded the title compound (60 mg, 54%) which was obtained as a light yellow foam. MS: m/e=364.5 [M+H]+.

1. additionwas added
2. stirringThe reaction mixture was stirred at 90° C. for 2 h
3. temperaturecooled to room temperature
4. extractionExtraction (ethyl acetate/saturated aqueous Seignette salt solution)
5. dry with materialby drying of the organic phase over sodium sulfate and evaporation
6. customafforded an oil
7. customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 0:100)