反应详情

温度

160 °C

Ammonium acetate (947 mg, 12.3 mmol) was added to an ambient temperature solution of tert-butyl 2-{[(4,4-dimethyl-2-oxohexyl)amino]carbonyl}-4,4-difluoro-2-[4-(5-fluoropyridin-2-yl)benzyl]pyrrolidine-1-carboxylate (138 mg, 0.25 mmol) in xylenes (10 mL). After stirring in a sealed tube at 160° C. for 1 h, the reaction mixture was diluted with ethyl acetate and water. The organic phase was dried (magnesium sulfate), filtered, and concentrated in vacuo. The residue was purified by chromatography over silica eluting with 0-100% ethyl acetate/hexane followed by high pressure liquid chromatography (KR100-5C18 100×21.2 mm column) eluting with 10-100% acetonitrile/water containing 0.05% trifluoroacetic acid. The residue was dissolved in trifluoroacetic acid (1 mL). After stirring at ambient temperature for 2 h, the reaction mixture was concentrated to afford the title compound. (M+H) found: 443.

1. dry with materialThe organic phase was dried (magnesium sulfate)
2. filtrationfiltered
3. concentrationconcentrated in vacuo
4. customThe residue was purified by chromatography over silica eluting with 0-100% ethyl acetate/hexane
5. washeluting with 10-100% acetonitrile/water containing 0.05% trifluoroacetic acid
6. dissolutionThe residue was dissolved in trifluoroacetic acid (1 mL)
7. stirringAfter stirring at ambient temperature for 2 h
8. concentrationthe reaction mixture was concentrated