4,4'-Dichloro-3,3'-dinitrobenzophenone → 3,3'-Diaminobenzophenone

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

To an autoclave there are added 50 g (0.15 moles) of 3,3'-dinitro-4,4'-dichloro benzophenone, 21 g (0.38 moles) of calcium oxide, 1 g of 5% palladium/alumina catalyst (available from Nihon-Engelhardt Co., Ltd.) and 350 ml of 1,2-dichloro ethane. The reaction is carried out for ten hours by introducing hydrogen into the autoclave, with the mixture being stirred at 30°-35° C., to keep the pressure at 10 Kg/cm2.G. After the completion of the reaction, the reaction mixture is heated up to 70° C. and subjected to a hot filtering so as to remove the catalyst and the inorganic salt. On cooling the mixture there are obtained yellow needle-like crystals of 3,3'-diamino benzophenone. The crystals are filtered, washed with 10 ml of 1,2-dichloro ethane and dried. Yield 21.2 g (67%). M.P. 149°-150.5° C. Recrystallization from ethanol gives pure crystals. M.P. 150°-151° C.

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