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ChemicalBook CAS DataBase List 3-TERT-BUTYL-4-HYDROXYANISOLE

3-TERT-BUTYL-4-HYDROXYANISOLE synthesis

12synthesis methods
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Yield:121-00-6 33.32%

Reaction Conditions:

with Na+-K+/MgO-CaO bimetallic basic catalyst at 170; under 9000.9 Torr; for 4 h;Autoclave;Temperature;Reagent/catalyst;

Steps:

1-17 Example 17
General procedure: In a high pressure reactor equipped with a condenser, the raw material TBHQ 332g was added to the reaction vessel and passed through a high purity N2 test.The airtightness of the autoclave was released. After the pressure was released, 3.3 g of a bimetallic basic catalyst and 90 g of dimethyl carbonate were added to the reaction vessel at a reaction temperature of 180 ° C. The maximum pressure during the reaction was maintained at 1.2 MPa, and the reaction time was 7.0 h. . After the reaction is completed, the temperature of the reaction vessel is lowered to room temperature by condensed water, and a small amount of the reaction liquid is taken in the sample tube, and after gas chromatography. In the case where the BHA synthesis process is identical to that of Example 1, the amount of catalyst is changed to 6.6 g, and the reaction time is changed. It was 4 h, and the reaction temperature was 170 ° C to obtain a reaction liquid of BHA. Quantitative analysis by gas chromatography showed that the conversion of TBHQ was 34%, the selectivity to 3-BHA was 98%, and the yield of BHA was 33.32%.

References:

Brethren Technology Co., Ltd.;Zhou Zhongping;Zhang Qiuhua;Wu Xiaole;Zhu Yuxiang CN108314609, 2018, A Location in patent:Paragraph 0022-0050

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