反应详情

To a solution of 2-amino-4-difluoromethyl-benzoic acid methyl ester (1.98 g, 9.84 mmol) in EtOH (75 mL) were added Ag2SO4 (3.08 g, 1 equiv) and I2 (2.50 g, 1 equiv) and the resulting mixture was stirred at r.t. for 1 hour. The mixture was filtered through a pad of celite and washed with EtOH. The solution was concentrated in vacuo and then diluted with AcOEt. The organic phase was washed with sat. aq NaHCO3, 1M aq Na2S2O3 and brine and dried (Na2SO4). The solution was concentrated in vacuo to afford the title compound as an off-white solid (2.9 g, 90% yield). ES-MS: m/z 369.2 [M+CH3CN+H]+, rt 5.87 min.

1. filtrationThe mixture was filtered through a pad of celite
2. washwashed with EtOH
3. concentrationThe solution was concentrated in vacuo
4. additiondiluted with AcOEt
5. washThe organic phase was washed with sat. aq NaHCO3, 1M aq Na2S2O3 and brine
6. dry with materialdried (Na2SO4)
7. concentrationThe solution was concentrated in vacuo