反应详情

To a closed glass vessel equipped with a thermometer and a stirrer, there are added 102 g (0.3 moles) of 3,3'-dinitro-4,4'-dichloro benzophenone, 5 g of 5% palladium/active carbon catalyst (available from Nihon Engelhardt Co.) and 300 ml of dioxane. While the mixture is being stirred at 70°-80° C., hydrogen is introduced in the vessel so that 41.5 l (1.85 moles) of hydrogen is absorbed into the mixture over 8 hours. After addition of 80 g (0.8 moles) of 40% aqueous sodium hydroxide, hydrogen is again introduced to the vessel with the mixture being stirred at 70°-80° C., so that it is absorbed 13.8 l (0.62 moles) over 3 hours. The reaction solution is filtered at 70°-80° C. to remove the catalyst. On cooling the solution, there is obtained 3,3'-diamino benzophenone, as yellow needle-like crystals. The crystals are filtered, washed with 30 ml of 50% aqueous solution of dioxane and dried. Yield 59.2 g (93%). M.P. 149°-151° C.

1. customTo a closed glass vessel equipped with a thermometer and a stirrer, there
2. customis absorbed into the mixture over 8 hours
3. additionis again introduced to the vessel with the mixture
4. stirringbeing stirred at 70°-80° C., so that it
5. customis absorbed 13.8 l (0.62 moles) over 3 hours
6. filtrationThe reaction solution is filtered at 70°-80° C.
7. customto remove the catalyst
8. temperatureOn cooling the solution