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ChemicalBook CAS DataBase List 3,5-Diisopropyl-4-hydroxybenzoic acid
13423-73-9

3,5-Diisopropyl-4-hydroxybenzoic acid synthesis

4synthesis methods
-

Yield:13423-73-9 78%

Reaction Conditions:

at 40 - 60;Microwave irradiation;

Steps:

3.1
(1) in 500 ml in the reaction bottle, to join the hydroxy benzoic acid 133g (0.89 μM), adding isopropanol 300g (5 μM), solid acid 50g, stirring to a solid uniform. In putting into ultrasonic reactor, and is additionally provided with a return device, the reaction temperature is 40 - 60 °C, ultrasonic power 500W, reaction 1 - 3h, reaction solution gradually changed from white to yellow, and then into orange red. Using HPLC (method and embodiment 1 the same) tracking the reaction conversion, the reaction to the hydroxy benzoic acid is less than 5% the following calculating the reaction is complete, stopping the reaction, filtering of the solid acid catalyst, the catalyst can be applied to the next reaction; the filter placed about 5 - 10 °C crystalline 6 - 10h, the crystal filter, 50 - 60 °C drying 6h, HPLC detection, impurities less than 0.1%, to obtain the intermediate 4 - hydroxy - 3, 5 - diisopropyl benzoic acid 154g, the yield is 78%.

References:

Li Hong;Zhejiang Jiuxu Pharmaceutical Co., Ltd.;Pan Ziguo;Zheng Fangjun;Zhang Jintao;Chen Jingfang;Fan Lingling CN106588576, 2017, A Location in patent:Paragraph 0092; 0093

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