反应详情

A suspension of 3-nitro-5-trifluoromethyl-1,2-phenylenediamine (0.560 g, 2.53 mmol) and oxalic acid (0.325 g, 2.58 mmol) in 2N HCl (8.5 mL) was refluxed for 6 h. The suspension was then cooled to r.t. and the solid filtered, washed with water (5.0 mL) and dried under vacuum to yield 0.502 (72%) of pure title compound as a yellow brown powder, m.p. 329°-332° C.; 1H NMR (DMSO-d6): 7.640 (s, 1H), 8.111 (s, 1H), 11.414 (s, 1H), 12.432 (1H).

1. temperaturewas refluxed for 6 h
2. filtrationthe solid filtered
3. washwashed with water (5.0 mL)
4. customdried under vacuum