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以季铵盐和氢氧化钠为原料,经Hofmann消除反应合成了[2,2]-对二甲苯环二体及其氯代物。考察了催化剂种类、反应物料摩尔比、反应温度、反应时间等因素对收率的影响。合成[2,2]-对二甲苯环二体的较优工艺条件为:苯醌为催化剂,n(NaOH):n(季铵盐)=5:1,120℃反应12h,[2,2]-对二甲苯环二体的收率为51.2%。合成氯代-[2,2]-对二甲苯环二体的较优工艺条件为:苯醌为催化剂,n(NaOH):n(季铵盐)=5:1,采用将氢氧化钠溶液滴入季铵盐的反滴工艺,110℃反应14h,氯代-[2,2]-对二甲苯环二体的收率为48.6%。用IR、1HNMR对产物结构进行了表征。
Using quaternary ammonium salt and sodium hydroxide as raw materials, [2,2] -p-xylene ring and its chlorides were synthesized by Hofmann elimination reaction. The effects of catalyst type, molar ratio of reactants, reaction temperature and reaction time on the yield were investigated. The optimum conditions for the synthesis of [2,2] -p-xylene ring are: benzoquinone as catalyst, n (quaternary ammonium salt) = 5: 1,120 ℃ for 12h, The yield of p-xylene ring was 51.2%. The optimum conditions for the synthesis of chloro- [2,2] -p-xylene ring are: benzoquinone as catalyst, n (NaOH): n (quaternary ammonium salt) = 5: 1, sodium hydroxide solution The dropping of the quaternary ammonium salt was carried out and the reaction was carried out at 110 ° C for 14h. The yield of chloro-2,2-para-xylene ring was 48.6%. The structure of the product was characterized by IR and 1HNMR.