反应详情

温度

0 °C

Stir a mixture of 3-[[4-(4-acetyl-3-hydroxy-2-propyl-phenoxymethyl)-phenyl]-(tetrahydro-pyran-2-yloxy)-methyl]-benzonitrile (13.4 g, 26.88 mmol), p-toluenesulfonic acid monohydrate (5.1 g, 26.88 mmol), methanol (100 mL), dichloromethane (50 mL), and ethyl acetate (50 mL) at room temperature for an hour. Concentrate the reaction mixture, dilute with ethyl acetate (150 mL) and wash with water (2×100 mL). Dry the organic phase over magnesium sulfate, filter, and concentrate. Dilute the residue with 5:1 hexanes:dichloromethane (50 mL), cool to 0° C. and filter. Collect a second and third crop to give the title compound (10.3 g, 93%), as a white solid. LCMS 416 M+1.

1. concentrationConcentrate the reaction mixture
2. additiondilute with ethyl acetate (150 mL)
3. washwash with water (2×100 mL)
4. dry with materialDry the organic phase over magnesium sulfate
5. filtrationfilter
6. concentrationconcentrate
7. additionDilute the residue with 5:1 hexanes
8. filtrationfilter
9. customCollect a second and third crop