反应详情

To a solution of isopropylamine (0.69 mL, 8 mmol) in dioxane (5 mL) was added dropwise trimethylaluminum solution (2M solution in hexane, 4 mL, 8 mmol). After stirring for 1 h at room temperature a suspension of 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid methyl ester (650 mg, 2 mmol) in dioxane (5 mL) was added. The reaction mixture was stirred at 90° C. for 90 min, 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 20:80) afforded the title compound (600 mg, 85%) as a white solid MS: m/e=352.3 [M+H]+.

1. additionwas added
2. stirringThe reaction mixture was stirred at 90° C. for 90 min
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 20:80)