2-羟基-3-叔丁基-5-甲基苄醇的制备及性能
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山西省自然科学基金(2015021045)


Preparation and Properties of 2-Hydroxy-3-tert-butyl-5-methylbenzyl Alcohol
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Natural Science Foundation of Shanxi Province (2015021045)

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    摘要:

    以2-叔丁基对甲酚、多聚甲醛为原料,乙二醇二甲醚和二甲苯为混合溶剂制备了2-羟基-3-叔丁基-5甲基苄醇。最优合成工艺条件为:反应温度为150℃,反应时间为20h,2-叔丁基对甲酚与多聚甲醛的物质的量比为1:20,2-叔丁基对甲酚与乙二醇二甲醚的物质的量比为1:1.5。采用熔点测试、FTIR、1HNMR、13CNMR、HRMS、单晶测试对合成产物进行了表征和结构确定,并采用HPLC对其纯度进行了分析,采用热重分析对其进行了热稳定性评价。对2-羟基-3-叔丁基-5-甲基苄醇进行了抗氧化性能测试,结果表明:2-羟基-3-叔丁基-5-甲基苄醇具有对超氧阴离子O3-、·OH自由基及DPPH·自由基较好的清除能力。

    Abstract:

    2-Hydroxy-3-tert-butyl-5-methylbenzyl alcohol has been synthesized using 2-tert-butyl-para-cresol and paraformaldehyde as raw materials with ethylene glycol dimethyl ether and xylene as mixed solvent. The optimum synthesis conditions of 2-hydroxy-3-tert-butyl-5-methylbenzyl alcohol were obtained: the reaction temperature was 150℃, the reaction time was 20h, The molar ratio of 2-tert-butyl-para-cresol to paraformaldehyde was 1:20 and the ratio of 2-tert-butyl-para-cresol to ethylene glycol dimethyl ether was 1:1.5. The synthetic product was characterized by melting point test, FTIR, 1HNMR, 13CNMR, HRMS and X-ray diffraction analysis. The purity the synthesized product was analyzed by HPLC. The thermal stability was also investigated by using thermogravimetric analysis (TGA). The antioxidant properties of the synthesized 2-hydroxy-3-tert-butyl-5-methylbenzyl alcohol were tested. The results showed that the product had good scavenging ability to superoxide O3-· anion, ·OH and DPPH· radical.

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王立敏.2-羟基-3-叔丁基-5-甲基苄醇的制备及性能[J].精细化工,2019,36(8):

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  • 收稿日期:2019-01-02
  • 最后修改日期:2019-03-23
  • 录用日期:2019-03-25
  • 在线发布日期: 2019-07-10
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