反应详情

温度

-30 °C

To a solution of 5-fluoro-2-(2-fluoro-4-trimethylsilanyl-phenylamino)-6-formylaminomethyl-nicotinic acid methyl ester (2.6 g, 6.6 mmol) in dichloromethane (65 mL) at −30° C. was added NBS (1.2 g, 6.6 mmol). The reaction mixture was stirred at −30° C. for 1.5 hours, and then concentrated under reduced pressure The resultant residue was taken up in ethyl acetate and this organic solution was washed with a saturated aqueous solution of sodium bicarbonate, followed by brine, dried (Na2SO4), filtered and evaporated in vacuo to afford the title compound as a brown solid (2.49 g, 95%). LCMS (method B): RT=3.79 min, [M+H]+=400/402.

1. concentrationconcentrated under reduced pressure The resultant residue
2. washthis organic solution was washed with a saturated aqueous solution of sodium bicarbonate
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated in vacuo