Calixarene phosphate derivative with upper edge full eliminated and lower edge full substituted and preparation method of derivative
An arene phosphate and derivative technology, which is applied in the field of functionalized modified calixarene phosphate derivatives, can solve the problems of low yield, complex synthesis route, incomplete derivative substitution, etc., and achieves high reaction yield, The synthetic route is simple and the effect of substitution is complete
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Embodiment 1
[0029] Take 4 g of p-tert-butylcalixarene, 2.72 g of phenol, and 5.22 g of anhydrous aluminum trichloride, put them in a 250 mL double-necked round bottom flask, and pour 60 mL of toluene. Stir on a magnetic stirrer, and react for 1 h under the protection of N2. The color of the mixture changed from colorless turbid liquid to orange turbid liquid. Pour the mixture into 100mL 0.2mol·L -1 hydrochloric acid solution, separated the white jelly in the upper layer through a separatory funnel, placed it in a round bottom flask, and evaporated to obtain a white solid, which was washed with acetone, methanol, chloroform, and ether in sequence, and the filter cake was dried to obtain an off-white solid. The intermediate product goes to tert-butylcalixarene. The yield is 96%, and its product purity is greater than 98%.
[0030] Take 4g (3mmol) of the synthesized intermediate product des-tert-butylcalixarene, 8.58g (60mmol) dimethyl chlorophosphate, 0.4g tetrabutylammonium bromide (TBA...
Embodiment 2
[0033] The synthesis method is similar to that of Example 1. Take 4 g of p-tert-butylcalixarene, 2.72 g of phenol, and 5.22 g of anhydrous aluminum trichloride, put them in a 250 mL double-necked round bottom flask, and pour 60 mL of toluene. Stir on a magnetic stirrer, and react for 1 h under the protection of N2. The color of the mixture changed from colorless turbid liquid to orange turbid liquid. Pour the mixture into 100mL 0.2mol·L -1 hydrochloric acid solution, separated the white jelly in the upper layer through a separatory funnel, placed it in a round bottom flask, and evaporated to obtain a white solid, which was washed with acetone, methanol, chloroform, and ether in sequence, and the filter cake was dried to obtain an off-white solid. The intermediate product goes to tert-butylcalixarene. The yield is 96%, and its product purity is greater than 98%.
[0034] Take 4g (3mmol) of the synthesized intermediate product de-tert-butylcalixarene, 10.32g (60mmol) diethyl ...
Embodiment 3
[0036] The synthesis method is similar to that of Example 1. Take 4 g of p-tert-butylcalixarene, 2.72 g of phenol, and 5.22 g of anhydrous aluminum trichloride, put them in a 250 mL double-necked round bottom flask, and pour 60 mL of toluene. Stir on a magnetic stirrer, and react for 1 h under the protection of N2. The color of the mixture changed from colorless turbid liquid to orange turbid liquid. Pour the mixture into 100mL 0.2mol·L -1hydrochloric acid solution, separated the white jelly in the upper layer through a separatory funnel, placed it in a round bottom flask, and evaporated to obtain a white solid, which was washed with acetone, methanol, chloroform, and ether in sequence, and the filter cake was dried to obtain the intermediate product Off-white solid des-tert-butylcalixarene. The yield is 96%, and its product purity is greater than 98%.
[0037] Take 4g (3mmol) intermediate product de-tert-butylcalixarene, 12g (60mmol) diethyl chlorophosphate, 0.4g tetrabuty...
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