反应详情

温度

0 °C

3,4,5-Trichloroaniline (1.6 g, 11.2 mmol) was dissolved in water (4 mL), cooled to 0° C., conc. HCl (1.5 ml) followed by a solution of NaNO2 (0.7 g, 11.2 mmol) in water (4 mL), was added dropwise and the resulting mixture was stirred for 30 min. followed by the addition of a solution of 2-oxocyclohexanecarboxylic acid. The reaction mixture was warmed to room temperature and stirred for 1 h during which time a solid precipitated out which was filtered and air dried to give the title compound (1.0 g, 29%). 1H NMR (500 MHz, CDCl3, δ in ppm) 13.5 (bs, 1H), 7.26 (s, 2H), 2.70 (s, 2H), 2.53 (s, 2H), 1.87 (s, 4H).

1. additionwas added dropwise
2. temperatureThe reaction mixture was warmed to room temperature
3. stirringstirred for 1 h during which time a solid
4. customprecipitated out which
5. filtrationwas filtered
6. customair dried