反应详情

A mixture of 4,6-dimethyl-2-nitroaniline (10.0 g, 60.2 mmol) and 10% Pd/C (1.0 g) in EtOH (300 mL) was stirred under an atmosphere of hydrogen (ca. 1 atm) for 3 h, then filtered through a celite pad and concentrated in vacuo. The crude solid was dissolved in CH3CN (200 mL) and triphosgene (15.0 g, 50.5 mmol) was added. The mixture was stirred for 1 h, then H2O (200 mL) was added slowly and stirring was continued for 1 h. The precipitate was isolated by filtration and dried to give the title compound. MS: m/z=163 (M+1).

1. filtrationfiltered through a celite pad
2. concentrationconcentrated in vacuo
3. dissolutionThe crude solid was dissolved in CH3CN (200 mL)
4. stirringThe mixture was stirred for 1 h
5. stirringstirring
6. waitwas continued for 1 h
7. customThe precipitate was isolated by filtration
8. customdried