反应详情

温度

95 °C

A mixture of 5-acetyl-2-(4-bromo-2-chlorophenylamino)-3,4-difluorobenzoic acid methyl ester (288 mg, 0.688 mmol) and formamidine acetate (77 mg, 0.74 mmol) in DMA (7 mL) was heated for 4 hours at 95° C. Additional 10 mg (0.096 mmol) of formamidine acetate was added and the reaction mixture was heated for additional 4 hours at 95° C. The reaction mixture was diluted with EtOAc, and washed with water (3×). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to give the crude material which was purified by silica gel flash column chromatography (100% CH2Cl2 to 1% MeOH in CH2Cl2) to afford the desired product (140 mg, 48%).

1. temperaturethe reaction mixture was heated for additional 4 hours at 95° C
2. washwashed with water (3×)
3. dry with materialThe organic layer was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto give the crude material which
7. customwas purified by silica gel flash column chromatography (100% CH2Cl2 to 1% MeOH in CH2Cl2)