反应详情

A mixture of 2-amino-4-(1,1-difluoro-ethyl)-benzoic acid methyl ester (1.3 g, 6.04 mmol), I2 (1.53 g, 6.03 mmol) and Ag2SO4 (1.89 g, 6.03 mmol) in EtOH (40 mL) was stirred for 1 h at r.t. The suspension was then filtered and the filtrate diluted with EtOAc and washed once with a 10% aqueous Na2SO3. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo to give 2-amino-4-(1,1-difluoro-ethyl)-5-iodo-benzoic acid methyl ester (1.98 g, 5.8 mmol, 96%) as a brown solid, ESI-MS: m/z 383 [M+CH3CN+H]+. rt 6.71 min

1. filtrationThe suspension was then filtered
2. additionthe filtrate diluted with EtOAc
3. washwashed once with a 10% aqueous Na2SO3
4. dry with materialThe organic layer was dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo