反应详情

温度

80 °C

Dissolve tetrabutylammonium fluoride trihydrate (0.436 g, 1.36 mmol) in 5 ml of acetonitrile. Add water (0.05 ml. 2.72 mmol) and stir for 10 minutes. Add trans-methanesulfonic acid 4-{(R)-3-[3,5-dichloro-4′-(4-trifluoromethyl-piperidine-1-carbonyl)-biphenyl-4-ylmethyl]-2-oxo-pyrrolidin-1-yl}-cyclohexyl ester (0.458 g, 0.68 mmol). Stir at 80° C. for 12 hours. Quench with saturated aqueous sodium bicarbonate and extract with ethyl acetate. Wash the extract with brine. Dry the organic layer over magnesium sulfate, filter, and concentrate under vacuum. Purify by silica gel chromatography recover 0.036 g (9%) of the title compound: MS (m/z): 579 (M+).

1. customQuench with saturated aqueous sodium bicarbonate
2. extractionextract with ethyl acetate
3. washWash the
4. extractionextract with brine
5. dry with materialDry the organic layer over magnesium sulfate
6. filtrationfilter
7. concentrationconcentrate under vacuum
8. customPurify by silica gel chromatography
9. customrecover 0.036 g (9%) of the title compound