反应详情

To a solution of 11.1 g 2,2-dimethyl-N-(2-methylphenyl) hydrazine carboxamide dissolved in 600 mL methylene chloride under N2 was added 17.1 g triphosgene. The solution was heated at reflux overnight, cooled, then concentrated under reduced pressure. The resulting residue was dissolved in ethyl acetate and washed with water, then saturated aqueous NaCl. The organic phase was dried (MgSO4), filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography (30-50% ethyl acetate/hexanes as eluent) to afford 8.25 g (64%) of the title compound of Step B. 1H NMR (CDCl3) δ 7.42-7.30 (m,3H), 7.17 (d,1H), 3.54 (s,3H), 2.22 (s,3H).

1. temperatureThe solution was heated
2. temperatureat reflux overnight
3. temperaturecooled
4. concentrationconcentrated under reduced pressure
5. dissolutionThe resulting residue was dissolved in ethyl acetate
6. washwashed with water
7. dry with materialThe organic phase was dried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by flash chromatography (30-50% ethyl acetate/hexanes as eluent)