反应详情

温度

100 °C

A mixture of 1-[5-(tert-Butyldiphenylsilanyloxymethyl)-4-[(2R,6S)-2,6-dimethyl-morpholin-4-yl]-2,3-difluorophenyl]ethanone (Intermediate 9, 0.5 g, 0.92 mmol), sulfur powder (0.06 g, 1.8 mmol), potassium iodide (0.08 g, 0.4 mmol) and 25% aqueous ammonia solution (10 mL) in DMSO (10 mL) was heated in a sealed tube at 100° C. for 4 hours. The reaction mixture was cooled and water was added. The mixture was extracted with ethyl acetate, which was dried (Na2SO4) and concentrated. The residue was purified by column chromatography (1:9 ethyl acetate:hexanes) to afford product as a yellow solid. Yield: 0.18 g (63%).

1. temperatureThe reaction mixture was cooled
2. extractionThe mixture was extracted with ethyl acetate, which
3. dry with materialwas dried (Na2SO4)
4. concentrationconcentrated
5. customThe residue was purified by column chromatography (1:9 ethyl acetate:hexanes)
6. customto afford product as a yellow solid