3,5-二叔丁基-4-羟基苄基甲醚的合成及表征

以2,6-二叔丁基酚和多聚甲醛为主要原料,二乙胺为催化剂,在甲醇中加热反应生成了3,5-二叔丁基- 4-羟基苄基甲醚。研究了催化剂的种类和加入量、反应物料配比、反应温度、反应时间、结晶温度等对产物收率的影响。结果表明,以150 g 2,6-二叔丁基苯酚为基准,催化剂用量为2,6-二叔丁基苯酚质量的5%,聚甲醛30 g,甲醇550 mL,反应温度130℃,反应时间6 h,收率达到90%,纯度为97%,用甲醇重结晶后纯度达到99.5%以上。通过FT-IR、~1H NMR和HPLC对其结构进行了表征。

SYNTHESIS AND CHARACTERIZATION OF 3,5-DI-tert-BUTYL-4-HYDROXYLBENZYL METHYL ETHER

3,5-Di-tert-butyl-4-hydroxylbenzyl methyl ether,an important intermediate of the antioxidant 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl) benzene,was efficiently synthesized by reacting 2,6-di-tert-butylphenol with paraformaldehyde and methanol in the presence of dimethylamine as catalyst.Effects of catalysts,reactant ratios,reaction temperature,reaction time and crystallization temperature on the yield were investigated.The optimum reaction conditions were found as follows:2,6-di-tert-butylphenol 150 g,methanol 550 mL,dimethylamine:2,6-di-tert-butyl-phenol =0.05:1(mass ratio),paraformaldehyde 30 g,reaction time 6 h,reaction temperature 130℃and crystallization temperature 10℃.Under the optimum conditions,the yield and purity of 3,5-di-tert -butyl-4-hydroxylbenzyl methyl ether was 90%and 97%,respectively.After recrystallization with methanol,the purity was above 99.5%.The product was characterized by FTIR,~1H NMR and HPLC.