反应详情

2-Methoxy-1,3-dinitro-5-trifluoromethylbenzene (3.0 g, 11.3 mmol) was dissolved in 100 mL 50:50 EtOAc:MeOH. Ammonium formate (7.06 g, 112 mmol) was added followed by palladium-on-carbon catalyst (1.0 g). The reaction was heated to a gentle reflux for 45 min, then allowed to cool, and filtered through a plug of diatomaceous earth. The calalyst was washed with EtOAc repeatedly, and the filtrate was in vacuo. The residue was taken up in 500 ml 50% EtOAc in hexanes and filtered through a short plug of silica gel. The filtrate was concentrated in vacuo, providing 2.15 g (10.4 mmol, 95%) of 2-methoxy-5-trifluoromethyl-benzene-1,3-diamine as a brown oil.

1. temperatureThe reaction was heated to
2. temperaturea gentle reflux for 45 min
3. temperatureto cool
4. filtrationfiltered through a plug of diatomaceous earth
5. washThe calalyst was washed with EtOAc repeatedly
6. filtrationfiltered through a short plug of silica gel
7. concentrationThe filtrate was concentrated in vacuo