Реакция #324366

Уравнение реакции

1,2,4,5-cyclohexanetetracarboxylic acid

acetic anhydride

→

1,2,4,5-cyclohexanetetracarboxylic dianhydride

Выход 96.7%

Условия реакции

Обработка

1. 1
   Другоеequipped with a Dimroth condenser
2. 2
   ТемператураThe temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
3. 3
   Температураto reflux for 10 min
4. 4
   Другоеwas decreased to room temperature
5. 5
   workup.STIRRINGunder stirring
6. 6
   Другоеto precipitate crystals
7. 7
   ДругоеThe precipitated crystals were separated by solid-liquid separation
8. 8
   Другоеdried
9. 9
   Другоеto obtain primary crystals
10. 10
    ДругоеThe mother liquor after separation
11. 11
    Концентрированиеwas concentrated under reduced pressure
12. 12
    Другоеa rotary evaporator
13. 13
    Другоеto precipitate crystals
14. 14
    ДругоеThe precipitated crystals were separated by solid-liquid separation
15. 15
    Другоеdried
16. 16
    Другоеto obtain secondary crystals

Методика

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%).

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