反应详情

A solution of 6-aminomethyl-2-(2-fluoro-4-trimethylsilanyl-phenylamino)-nicotinic acid methyl ester (13.2 g, 38.2 mmol) in formic acid (200 mL) and acetic anhydride (40 mL) was stirred at ambient temperature for 1 hour. The reaction mixture was concentrated in vacuo and the residue azeotroped with toluene. The resultant residue was dissolved in dichloromethane and washed with a saturated aqueous solution of sodium, hydrogen carbonate, followed by brine. The organic phase was isolated, dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound as a yellow solid (12.7 g, 89%). LCMS (method B): RT=4.17 min, M+H+=376.

1. concentrationThe reaction mixture was concentrated in vacuo
2. customthe residue azeotroped with toluene
3. dissolutionThe resultant residue was dissolved in dichloromethane
4. washwashed with a saturated aqueous solution of sodium, hydrogen carbonate
5. customThe organic phase was isolated
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo