Preparation method of mono-tert-butyl glutarate
A technology of mono-tert-butyl ester and glutaric acid, which is applied in the field of compound synthesis, can solve the problems of harsh reaction conditions and low product yield, and achieve the effect of simple method, high product yield, and reduction of operational safety hazards
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Embodiment 1
[0026] The preparation method of the mono-tert-butyl glutarate of the present embodiment may further comprise the steps:
[0027] Under the condition of air, add 1.71g of anhydrous zinc chloride and 143mL of tert-butanol to the reactor equipped with a thermometer, agitator and condenser, and stir at 25°C until it becomes a white emulsion. After stirring for 1h, Add 28.8g of glutaric anhydride to the reactor, raise the temperature to 50°C for the first step reaction, cool down to 25°C after the first step for 20 hours, add 67.2g of glutaric anhydride to the reactor, raise the temperature to 70°C The second step of reaction, the second step of reaction for 28 hours, TLC detection to confirm the end of the reaction, the reactor was naturally cooled to 25 ° C, and then the temperature was programmatically cooled to -20 ° C, after 15 hours of heat preservation, the filtrate was filtered while cold, and the filter residue was washed with ice petroleum ether , and the combined filtra...
Embodiment 2
[0030] The preparation method of the mono-tert-butyl glutarate of the present embodiment may further comprise the steps:
[0031] Under the condition of air, add 1.15g of anhydrous zinc chloride and 96mL of tert-butanol to the reactor equipped with a thermometer, agitator and condenser, and stir at 30°C until it becomes a white emulsion. After stirring for 3 hours, Add 28.8g of glutaric anhydride to the reactor, raise the temperature to 40°C for the first step reaction, after the first step of reaction for 20h, cool down to 20°C, add 67.2g of glutaric anhydride to the reactor, raise the temperature to 55°C The second step of reaction, the second step of reaction for 49 hours, TLC detection to confirm the end of the reaction, the reactor was naturally cooled to 25 ° C, and then the temperature was programmatically cooled to -30 ° C, after 18 hours of heat preservation, the filtrate was filtered while cold, and the filter residue was washed with ice petroleum ether , and the com...
Embodiment 3
[0033] The preparation method of the mono-tert-butyl glutarate of the present embodiment may further comprise the steps:
[0034] In the air, add 3.45g of anhydrous zinc chloride and 240.6mL of tert-butanol to the reactor equipped with a thermometer, stirrer and condenser, and stir at 20°C until it becomes a white emulsion. After stirring for 2 hours, , add 28.8g of glutaric anhydride to the reactor, raise the temperature to 55°C for the first step of reaction, after the first step of reaction for 12 hours, cool down to 30°C, add 67.2g of glutaric anhydride to the reactor, and raise the temperature to 80°C Carry out the second step reaction, the second step reaction is 23h, TLC detection confirms the reaction end point, the reactor is naturally cooled to 25°C, and then the temperature is programmatically cooled to 0°C, after 12h of heat preservation, the filtrate is filtered while cold, and the filter residue is washed with ice petroleum ether , and the combined filtrate was c...
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