Azane;hydrate → 3,3'-Diaminobenzophenone

Participants

Reaction Conditions

Reaction Steps

Then, in a closed glass vessel with a thermometer and a stirrer, there are charged 34 g (0.1 moles) of said crude dinitro-dichloro benzophenone, 1 g of 5% Pd/C and 100 ml of methyl cellosolve. While stirring the mixture, at 40°-50° C., there is introduced hydrogen so that 13.9 l (0.62 moles) of hydrogen is absorbed in the mixture during twelve hours. Then, the mixture is cooled down to 30° C. and added with 18.2 g (0.3 moles) of 28% ammonia water. There is introduced hydrogen, with the mixture being stirred at 30°-35° C., so that 4.3 l (0.19 moles) of hydrogen is absorbed during five hours. After completion of reaction, the mixture is heated up to 70° C. for hot filtering to remove the catalyst. After being added with 100 ml of hot water, the filtrate is allowed to cool to give yellow crystals of 3,3'-diamino benzophenone. The crystals are filtered, washed with 10 ml of ethanol and dried. Yield 16.8 g (79.2%). M.P. 148°-150° C. Recrystallization from ethanol yields slightly yellow needle-like crystals of the diamino benzophenone. M.P. 150° to 151° C.

Provenance & Evidence