反应详情

To a closed glass vessel equipped with a thermometer and a stirrer, there are added 49 g (0.15 moles) of 3,3'-dinitro-4-chloro-4'-fluoro benzophenone, 1 g of palladium black catalyst and 300 ml of benzene. While the mixture being stirred at 65°-70° C., 20.2 l (0.9 moles) of hydrogen is absorbed therein during about 6 hours. Then, after there are added 180 g (0.45 moles) of 35% aqueous solution of potassium carbonate and 3 g of 90% aqueous solution of trioctylmethyl ammonium chloride (available from Tokyo-Kasei Co.), additional hydrogen, 7.4 l (0.33 moles), is introduced during about 5 hours while the mixture being stirred at 65°-70° C. The mixture at that temperature is filtered to remove the catalyst. Organic phase is separated from the filtrate, added with magnesium sulfate for removing water and then blown with dry hydrochloric gas to saturation. The precipitate thus obtained is filtered, washed with 50 ml of benzene and dried to obtain 33.2 g (yield 77.7%) of 3,3'-diamino benzophenone in the hydrochloric acid salt form. Recrystallization from 20% aqueous isopropyl alcohol gives pure compound, as slightly yellow needle-like crystals. M.P. 265°-267° C. (decomposed).

1. customTo a closed glass vessel equipped with a thermometer and a stirrer, there
2. additionis introduced during about 5 hours while the mixture
3. stirringbeing stirred at 65°-70° C
4. filtrationThe mixture at that temperature is filtered
5. customto remove the catalyst
6. customOrganic phase is separated from the filtrate
7. additionadded with magnesium sulfate
8. customfor removing water
9. customwith dry hydrochloric gas to saturation
10. customThe precipitate thus obtained
11. filtrationis filtered
12. washwashed with 50 ml of benzene
13. customdried