반응 #324366

반응 방정식

1,2,4,5-cyclohexanetetracarboxylic acid

acetic anhydride

→

1,2,4,5-cyclohexanetetracarboxylic dianhydride

수율 96.7%

반응 조건

후처리

1. 1
   기타equipped with a Dimroth condenser
2. 2
   온도The temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
3. 3
   온도to reflux for 10 min
4. 4
   기타was decreased to room temperature
5. 5
   workup.STIRRINGunder stirring
6. 6
   기타to precipitate crystals
7. 7
   기타The precipitated crystals were separated by solid-liquid separation
8. 8
   기타dried
9. 9
   기타to obtain primary crystals
10. 10
    기타The mother liquor after separation
11. 11
    농축was concentrated under reduced pressure
12. 12
    기타a rotary evaporator
13. 13
    기타to precipitate crystals
14. 14
    기타The precipitated crystals were separated by solid-liquid separation
15. 15
    기타dried
16. 16
    기타to obtain secondary crystals

실험 절차

Subsequently, 450 g of the obtained 1,2,4,5-cyclohexanetetracarboxylic acid and 4,000 g of acetic anhydride were charged into a 5-L glass separable flask equipped with a Dimroth condenser. The inner atmosphere of the reactor was replaced with nitrogen gas under stirring. The temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere to allow the solvent to reflux for 10 min. After that, the temperature was decreased to room temperature under stirring to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain primary crystals. The mother liquor after separation was concentrated under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain secondary crystals. In total of the primary and secondary crystals, 375 g of 1,2,4,5-cyclohexanetetracarboxylic dianhydride was obtained (yield of the dianhydride: 96.6%).

출처