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ChemicalBook CAS DataBase List 4-tert-Butylbenzoic acid

4-tert-Butylbenzoic acid synthesis

13synthesis methods
-

Yield:98-73-7 99.3%

Reaction Conditions:

with oxygen;nitric acid at 120; for 0.0833333 h;

Steps:

9

General procedure: Open the bottom valve of the p-nitrotoluene storage tank and the bottom valve of the nitric acid storage tank, put the raw material p-nitrotoluene and 30% nitric acid into the upper tank 3 and mix them uniformly. The ratio of nitric acid to p-nitrotoluene is 5 :1. Turn on the feed pump, control the flow rate to 200Kg/h, make the residence time of the reaction liquid in the loop reactor be 300s, turn on the loop reactor 6, make the small diameter sleeve 62 rotate at 1000 rpm, turn on the oxygen Inlet gas, the purity of oxygen is 99.0%; the temperature control system is turned on, and the heat transfer oil enters the heat exchange jacket 64 of the small diameter sleeve 62 and the large diameter sleeve 61 to heat the reaction liquid. After reaching the reaction temperature of 190°C, the temperature control system will keep the reaction temperature of the system at 190±5°C to make the system react steadily. After the system produces qualified products, put the reaction liquid into the crystallization kettle (5) 1. After the filling factor of the crystallization kettle (5) reaches 70%, switch to the crystallization kettle (5) two and the crystallization kettle (5) one side The temperature is lowered while stirring, and after the temperature is lowered to 80-85°C, it is placed in an automatic centrifuge for centrifugation, cleaning, drying, and then sent to packaging. The purity of the liquid phase is 99.9%, and the molar yield is 99.1%.

References:

CN113636928,2021,A Location in patent:Paragraph 0032-0033; 0035

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