反应详情

温度

70 °C

A mixture of 5-fluoro-3-methyl-2-nitrobenzoic acid (4.86 g, 24.42 mmol) and SnCl2 (16.5 g, 72.36 mmol) in EtOAc was heated at 70° C. overnight. After cooling at rt, the pH was adjusted to 7-8 with satd. aq. NaHCO3. The mixture was extracted with EtOAc, and the organic layer was washed with brine, filtered through diatomaceous earth, and dried over Na2SO4 to provide the title compound, which was used without further purification. ESI-MS (m/z): 170 [M+1]+.

1. temperatureAfter cooling at rt
2. extractionThe mixture was extracted with EtOAc
3. washthe organic layer was washed with brine
4. filtrationfiltered through diatomaceous earth
5. dry with materialdried over Na2SO4