反应详情

To a solution of 5-methyl-3-(tetrahydro-pyran-4-yl)-isoxazole-4-carboxylic acid ethyl ester (4.0 g, 16.7 mmol) in THF (55 mL) at 0° C. was added lithium aluminum hydride (349 mg, 9.0 mmol). And the resulting mixture stirred for 18 h at room temperature. Water (0.5 mL) was added carefully followed by aqueous sodium hydroxide (15%, 1.0 mL) and water (2.2 mL). The resulting suspension was stirred for 15 min at ambient temperature and filtered over Hyflo®. The filtrate was then evaporated and purification by chromatography (silica, heptane:ethyl acetate=100:0 to 1:1) afforded the title compound (1.1 g, 34%) as a colourless gum. MS: m/e=198.1 [M+H]+.

1. stirringThe resulting suspension was stirred for 15 min at ambient temperature
2. filtrationfiltered over Hyflo®
3. customThe filtrate was then evaporated
4. custompurification by chromatography (silica, heptane:ethyl acetate=100:0 to 1:1)