反应详情

To a stirred solution of 5-hydroxy-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester (4.68 g, 30 mmol) and [5-methyl-3-(tetrahydro-pyran-4-yl)-isoxazol-4-yl]-methanol (5.92 g, 30 mmol) in THF (400 mL) at 5° C. under argon was added triphenylphosphine (10.6 g, 39 mmol), then diisopropyl azodicarboxylate (8.23 mL, 39 mmol) was added dropwise. The reaction mixture was warmed to room temperature overnight. The reaction mixture was then extracted with ethyl acetate and the organic extract washed with water, dried over sodium sulphate, filtered and evaporated. Purification by chromatography (silica, heptane:ethyl acetate=1:1) afforded the title compound (7.26 g, 85%) as a white solid. MS: m/e=336.2 [M+H]+.

1. extractionThe reaction mixture was then extracted with ethyl acetate
2. extractionthe organic extract
3. washwashed with water
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated
7. customPurification by chromatography (silica, heptane:ethyl acetate=1:1)