Compound trimellitic anhydride n-heptyl ester and synthetic method thereof
A technology of trimellitic anhydride and trimellitic anhydride acid chloride is applied to the compound trimellitic anhydride n-heptyl ester and its synthesis field.
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Embodiment 1
[0026] A kind of compound trimellitic anhydride n-heptyl ester, its molecular structural formula is as follows:
[0027]
[0028] The synthetic method of above-mentioned compound trimellitic anhydride n-heptyl ester, concrete steps are as follows:
[0029] (1) Take trimellitic anhydride acid chloride, n-heptanol, and potassium carbonate in a molar ratio of 1:1.5:1.3; the amount of solvent petroleum ether is 5 times the volume of the reactant;
[0030] Put the weighed trimellitic anhydride acid chloride into the solvent petroleum ether, start the magnetic stirrer, first dissolve the trimellitic anhydride acid chloride in the petroleum ether, then place the weighed n-heptanol in a dropper, slowly drop it within 20 minutes, and obtain the reaction solution; Put potassium carbonate into the above reaction solution, then control the reaction temperature at -5-0°C, and react for 5 hours. The resulting solution is white, which is the crude product of n-heptyl trimellitic anhydride...
Embodiment 2
[0038] The synthetic method of compound trimellitic anhydride n-heptyl ester, concrete steps are as follows:
[0039] (1) Prepare ice salt according to the mass ratio of ice: sodium chloride = 100:23, and take trimellitic anhydride acid chloride, n-heptanol, and pyridine in a molar ratio of 1:0.9:1.5; the amount of solvent 1,2-dichloroethane is the reaction 7 times the volume of the object;
[0040] Put the weighed trimellitic anhydride acid chloride into the solvent dimethyl sulfoxide, start the magnetic stirrer, first dissolve the trimellitic anhydride acid chloride in dimethyl sulfoxide, then place the weighed n-heptanol and pyridine in the dropper, shake well, Slowly drop into the reaction system within 40min, then control the reaction temperature to -5~0°C (the reaction is carried out in an ice-salt bath environment to maintain the low temperature required for the reaction), react for 4h, the reaction system is white paste, and trimellitic anhydride is obtained. Heptyl e...
Embodiment 3
[0044] The synthetic method of compound trimellitic anhydride n-heptyl ester, concrete steps are as follows:
[0045] (1) According to the mass ratio of ice:ammonium nitrate=100:8, ice salt is prepared, and trimellitic anhydride acid chloride, n-heptanol, and potassium carbonate are taken in a molar ratio of 1:1:1.8; 8 times;
[0046] Put the weighed trimellitic anhydride acid chloride into the solvent dichloromethane, start the magnetic stirrer, first dissolve the trimellitic anhydride acid chloride in the dichloromethane, then place the weighed n-heptanol in the dropper, drop it slowly within 15min, and obtain the reaction Liquid; Potassium carbonate was put into the above reaction solution in portions within 30 minutes, the reaction temperature was controlled at -5 ~ 0 ° C, and the reaction was carried out for 3 hours. The resulting solution was white, which was the crude product of n-heptyl trimellitic anhydride.
[0047] (2) Impurity removal treatment: add an equal volum...
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Abstract
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