反应详情

A mixture of 10 g (60 mmol) of 4-(trifluoromethyl)-1,2-phenylenediamine (Lancaster) and 50 mL of formic acid was refluxed for 2 h. Excess formic acid was then removed in vacuo. To the resultant concentrate was added 200 mL of water during which time a precipitate was discerned. This was filtered and discarded. The filtrate was concentrated in vacuo and redissolved in EtOAc. After repeated washing with saturated NaHCO3, the EtOAc solution was dried over MgSO4 and concentrated. The concentrate was put on a vacuum pump overnight. This resulted in 9.27 g (83%) of a yellow solid. 1H NMR (DMSO-d6) δ7.5 (d,1H, aromatic), 7.8 (d, 1H, aromatic), 8 (s, 1H, aromatic), 8.4 (s, 1H, CH), 12.8 (br s, 1H, NH).

1. temperaturewas refluxed for 2 h
2. customExcess formic acid was then removed in vacuo
3. concentrationTo the resultant concentrate
4. additionwas added 200 mL of water during which time a precipitate
5. filtrationThis was filtered
6. concentrationThe filtrate was concentrated in vacuo
7. dissolutionredissolved in EtOAc
8. washAfter repeated washing with saturated NaHCO3
9. dry with materialthe EtOAc solution was dried over MgSO4
10. concentrationconcentrated
11. customwas put on a vacuum pump overnight