反应详情

To a degassed solution of 3-(2-fluoro-6-nitrophenylamino)propionic acid methyl ester from Example 1A (650 mg, 2.7 mmol) in methanol (40 ml) was added palladium on carbon (10%, 200 mg). Hydrogen gas was bubbled through the mixture for two hours, filtered through Celite® and reduced in vacuo. The residue was dissolved in propan-2-ol (20 ml) and to it was added acetic acid (2 ml). The mixture was stirred for 18 h, heated at reflux for 2 h, cooled, reduced in vacuo and azeotroped with toluene; yield 480 mg, 99%.

1. customHydrogen gas was bubbled through the mixture for two hours
2. filtrationfiltered through Celite®
3. dissolutionThe residue was dissolved in propan-2-ol (20 ml) and to it
4. additionwas added acetic acid (2 ml)
5. temperatureheated
6. temperatureat reflux for 2 h
7. temperaturecooled
8. customazeotroped with toluene