【摘要】 以叔丁醇为原料,优化了其与浓盐酸氯代合成叔丁基氯的反应,采用Ca Cl2氯化盐助催化体系使反应收率提高到95%,产品质量分数为99%;3,3-二甲基-1-丁烯合成的关键步骤是叔丁基氯与乙烯反应制备3,3-二甲基-1-氯丁烷,探讨了催化剂用量、反应温度对反应收率的影响。反应以无水三氯化铝为催化剂,用量为n(Al Cl3)∶n[(CH3)3CCl]=0.018∶1,反应温度为-17~-20℃时,产物3,3-二甲基-1-氯丁烷的收率可达80%;最后由3,3-二甲基-1-氯丁烷脱氯化氢制备3,3-二甲基-1-丁烯。考察了不同溶剂对反应收率的影响,以聚乙二醇-400为溶剂,无需加入相转移催化剂,收率可达88.5%,3,3-二甲基-1-丁烯的质量分数为可达95%以上。更多还原

【Abstract】 The tertiary butyl alcohol was chosen as a raw material to prepare 3,3-dimethyl-1-butene. The reaction conditions of tertiary butyl alcohol and concentrated hydrochloric acid were optimized. The yield was increased to 95% and the purity of product could reach 99% using 32% hydrochloric acid and Ca Cl2co-catalyst system. Then,the key-step of this method was the preparation of 1-chloro-3,3-dimethylbutane using tert-butyl chloride and ethylene. The influences of catalyst dosage and reaction temperature on the yield of product were investigated. The yield can be up to 85% when using anhydrous Al Cl3 as catalyst with catalyst dosage of n( Al Cl3) ∶ n(( CH3)3CCl) = 0. 018 ∶ 1 and the reaction temperature was- 20—- 17 ℃. Finally,the 3,3-dimethyl-1-butene was obtained by dehydrochlorination of 1-chloro-3,3-dimethylbutane. The impact of different solvents on the yield was studied. The results show that the best solvent is polyethylene glycol-400,which can improve the purity of product to more than 95% and the yield up to 88. 5% without phase transfer catalyst.更多还原