반응 #429506

반응 방정식

2,5-dicyano-1,4-dimethoxybenzene

aluminum tribromide

hydrochloric acid

→

2,5-dicyanohydroquinone

수율 41.7%

용매

benzene

반응 조건

후처리

1. 1
   온도by heat-refluxing for 7 hours
2. 2
   기타After the reaction
3. 3
   온도the reaction mixture as cooled
4. 4
   기타to precipitate a crystal
5. 5
   여과The crystal was recovered by filtration
6. 6
   workup.DISSOLUTIONdissolved in 2N-sodium hydroxide aqueous solution
7. 7
   여과The resultant insoluble residue was filtered off
8. 8
   기타to precipitate a crystal
9. 9
   여과The crystal was recovered by filtration
10. 10
    세척washed with water
11. 11
    기타by drying

실험 절차

In a 5 liter-reaction vessel, 100 g (5.32×10-1M) of 2,5-dicyano-1,4-dimethoxybenzene, 312.5 g (1.17M) of anhydrous aluminum tribromide and 2.5 liters of dry benzene were placed, followed by heat-refluxing for 7 hours. After the reaction, the reaction mixture as cooled and poured into a mixture of 3 kg of crushed ice and 500 ml of concentrated hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration and dissolved in 2N-sodium hydroxide aqueous solution. The resultant insoluble residue was filtered off and the filtrate was acidified with 2N-hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration and washed with water, followed by drying to obtain 35.5 g of 2,5-dicyanohydroquinone (Yield: 41.7%).

출처