反応 #324366

反応方程式

1,2,4,5-cyclohexanetetracarboxylic acid

acetic anhydride

→

1,2,4,5-cyclohexanetetracarboxylic dianhydride

収率 96.7%

反応条件

後処理

1. 1
   その他equipped with a Dimroth condenser
2. 2
   温度The temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
3. 3
   温度to reflux for 10 min
4. 4
   その他was decreased to room temperature
5. 5
   workup.STIRRINGunder stirring
6. 6
   その他to precipitate crystals
7. 7
   その他The precipitated crystals were separated by solid-liquid separation
8. 8
   その他dried
9. 9
   その他to obtain primary crystals
10. 10
    その他The mother liquor after separation
11. 11
    濃縮was concentrated under reduced pressure
12. 12
    その他a rotary evaporator
13. 13
    その他to precipitate crystals
14. 14
    その他The precipitated crystals were separated by solid-liquid separation
15. 15
    その他dried
16. 16
    その他to obtain secondary crystals

実験手順

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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