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Method for synthesizing p-tert-butyl calix [8] arene ester derivative

A technology of p-tert-butylcalix and tert-butylcalix, which is applied in the field of synthesizing p-tert-butylcalix[8]arene ester derivatives, can solve problems such as unfavorable research work, and facilitate industrial scale production and harvest. The effect of high efficiency and less impurities

Pending Publication Date: 2022-07-01
山东禹王工业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, its research work mainly focuses on p-tert-butylcalix[4]arene and its derivatives, while relatively little research is done on p-tert-butylcalix[8]arene and its derivatives, which is not conducive to the development of follow-up research work.

Method used

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  • Method for synthesizing p-tert-butyl calix [8] arene ester derivative
  • Method for synthesizing p-tert-butyl calix [8] arene ester derivative
  • Method for synthesizing p-tert-butyl calix [8] arene ester derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Dissolve 14.2 g of ethanol in 200.0 ml of chloroform, add 2.0 ml of triethylamine, and dropwise add 31.8 g of chloroacetyl chloride under stirring at room temperature. Solvent yields crude product. After the crude product was distilled under reduced pressure, an intermediate product Z1 was obtained; 20.0 g of p-tert-butyl calix[8] aromatic hydrocarbon and the intermediate product Z1 were dissolved in 500.0 ml of anhydrous acetone, 20.0 g of potassium carbonate and 3.0 g of potassium iodide were added, and nitrogen protection was carried out. Under reflux conditions (about 55°C), the reaction was carried out under reflux conditions, and the reaction progress was tracked by TLC. After the reaction was completed (about 12 hours of reaction), the insolubles were removed by suction filtration, and the solvent was spin-dried to obtain a crude product. The crude product was washed with methanol and recrystallized with ethanol-chloroform (v:v=5:1). Obtained final product A, 13...

Embodiment 2

[0046] Dissolve 18.5 g of n-propanol in 200.0 ml of chloroform, add 2.0 ml of triethylamine, and under stirring at room temperature, add 31.8 g of chloroacetyl chloride dropwise, react for 1 h, wash with distilled water three times, separate the liquid, and collect the organic phase , remove the solvent to get the crude product. After the crude product is distilled under reduced pressure, an intermediate product Z2 is obtained; 20.0 g of p-tert-butylcalix[8] arene and the intermediate product Z2 are dissolved in 500.0 ml of anhydrous acetone, 20.0 g of potassium carbonate and 3.0 g of potassium iodide are added, and nitrogen is protected. Under reflux conditions (about 55°C), the reaction was carried out under reflux conditions, and the reaction progress was tracked by TLC. After the reaction was completed (about 12 hours of reaction), the insolubles were removed by suction filtration, and the solvent was spin-dried to obtain a crude product. The crude product was washed with ...

Embodiment 3

[0048] 33.3 g of benzyl alcohol was dissolved in 200.0 ml of chloroform, 2.0 ml of triethylamine was added, 31.8 g of chloroacetyl chloride was added dropwise with stirring at room temperature, and after 1 h of reaction, washed with distilled water three times, separated, and the organic phase was collected. The crude product was obtained by removing the solvent. After the crude product was distilled under reduced pressure, an intermediate product Z3 was obtained; 20.0 g of p-tert-butyl calix[8] aromatic hydrocarbon, and the intermediate product Z3 were dissolved in 500.0 ml of anhydrous acetone, 20.0 g of potassium carbonate and 3.0 g of potassium iodide were added, and nitrogen protection was carried out. Under reflux conditions (about 55° C.), the reaction was carried out under reflux conditions, and the reaction progress was tracked by TLC. After the reaction was completed (about 12 hours of the reaction), the insolubles were removed by suction filtration, and the solvent w...

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Abstract

The invention relates to a method for synthesizing p-tert-butyl calix [8] arene ester derivatives, which comprises the following steps: 1) dissolving alcohol in an anhydrous aprotic organic solvent, adding an organic acid-binding agent, adding corresponding acyl chloride, and after the reaction is finished, washing with distilled water, separating liquid, removing the solvent, separating and purifying to obtain an intermediate product Z; and 2) dissolving p-tert-butyl calix [8] arene in an anhydrous aprotic organic solvent, adding an acid-binding agent and a catalyst, adding the intermediate product Z, after the reaction is finished, removing the acid-binding agent, the catalyst and the solvent, adding methanol, precipitating to obtain a crude product, and separating and purifying to obtain the final product p-tert-butyl calix [8] arene ester derivative. The p-tert-butyl calix [8] arene ester derivative is synthesized, calixarene, especially calix [8] arene derivative family is enriched, reaction conditions are mild, reaction steps are simple, the yield is high and can reach 65% or above, and industrial large-scale production is facilitated.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for synthesizing p-tert-butylcalix[8]arene ester derivatives. Background technique [0002] The information disclosed in this Background section is only for enhancement of understanding of the general background of the invention and should not necessarily be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. [0003] At present, most of the synthesis of calixarene is obtained by first preparing p-tert-butyl calixarene with p-tert-butylphenol and formaldehyde (including paraformaldehyde) under different reaction conditions, and then modifying it through various reactions. Therefore, the research on tert-butyl calixarene and its derivatization is of great significance to the whole research work of calixarene. At present, its research work mainly focuses on p-tert-butylcali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/736
CPCC07C67/14C07C67/31C07C2603/92C07C69/63C07C69/736
Inventor 王苒辛寅昌侯尔群张斌
Owner 山东禹王工业技术研究院有限公司
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