反应详情

温度

80 °C

A mixture of 1-(6-bromo-3-fluoro-4-triethylsilanyl-pyridin-2-yl)-2,2-difluoro-ethanone (9.8 g, 26.6 mmol), (S)-2-methylpropane-2-sulfinamide (3.23 g, 26.6 mmol) and tetraethoxytitanium (13.81 ml, 53.2 mmol) in THF (66.5 ml) was stirred at 80° C. in 3 capped microwave vials (3×25 ml) for 3 hours. The cold reaction mixture was poured into ice cold water and the precipitate was filtered through a pad of hyflo and washed thoroughly with ethyl acetate. The organic phase was washed with brine, dried over sodium sulfate, filtered and evaporated. The crude product (12.5 g) was chromatographed over silica gel (cyclohexane:ethyl acetate 5:1) to afford the title compound. 7.96 g (63% yield).

1. customThe cold reaction mixture
2. additionwas poured into ice cold water
3. filtrationthe precipitate was filtered through a pad of hyflo
4. washwashed thoroughly with ethyl acetate
5. washThe organic phase was washed with brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. customevaporated
9. customThe crude product (12.5 g) was chromatographed over silica gel (cyclohexane:ethyl acetate 5:1)