反应详情

温度

80 °C

A mixture of tert-butyl 4-{[(4-hydroxy-1,2-benzisoxazol-3-yl)oxy]methyl}piperidine-1-carboxylate (100 mg, 0.287 mmol, EXAMPLE 17, step 2), 1-oxaspiro[2.4]heptane (59.7 mg, 0.609 mmol), and potassium carbonate (156 mg, 1.13 mmol) in ethanol (2 mL) was heated at 80° C. for 5 h. After cooling to room temperature, the mixture was diluted with ethyl acetate (3 mL) and 5% aq. sodium chloride was added to the mixture. Organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated in vacuo to give a solid. The residual solid was purified by NH gel column chromatography (ethyl acetate/hexane 1:2) to give 95 mg (74%) of the title compound as a white solid.

1. temperatureAfter cooling to room temperature
2. additionwas added to the mixture
3. customOrganic layer was separated
4. washwashed with brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customto give a solid
8. customThe residual solid was purified by NH gel column chromatography (ethyl acetate/hexane 1:2)