반응 #94463

반응 방정식

Terephthaloyl dichloride

benzene

aluminum chloride

hydrochloric acid

→

1,4-Dibenzoylbenzene

반응 조건

후처리

1. 1
   온도The mixture is heated at 70° for 7 hours
2. 2
   온도cooled to 20°
3. 3
   온도maintained at this temperature for 18 hours with continual stirring
4. 4
   workup.ADDITIONThe reaction mixture is then added to 1 l
5. 5
   세척The benzene solution is washed three times with water
6. 6
   기타The excess benzene is removed by distillation
7. 7
   기타The resulting crystalline material is recrystallized from dimethylformamide, yield 22 g (76% of theory) white crystals mp 158°-9°

실험 절차

1,4-Dibenzoylbenzene is prepared essentially as described by Noelting and Kohn, Ber. 19, 147 (1886). Terephthaloyl dichloride (20.3 g, 0.1 mole) is dissolved in benzene (350 ml) and anhydrous aluminum chloride (30 g, 0.22 mole) is added. The mixture is heated at 70° for 7 hours, cooled to 20° and maintained at this temperature for 18 hours with continual stirring. The reaction mixture is then added to 1 l crushed ice and 20 ml 37% hydrochloric acid. The benzene solution is washed three times with water and twice with sodium bicarbonate solution. The excess benzene is removed by distillation. The resulting crystalline material is recrystallized from dimethylformamide, yield 22 g (76% of theory) white crystals mp 158°-9°.

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