标题化合物是聚羧酸减水剂聚醚大单体的关键起始剂,传统方法主要以直接水解或先酯化后水解两步法合成。利用甲代烯丙基氯和醋酸钠在相转移催化剂作用下合成为羧酸酯,直接加入30%的NaOH溶液水解,实现了标题化合物的"一锅法"绿色高效合成,收率均〉90%。利用核磁(1HNMR)、红外光谱和质谱(LRMS)表征了其结构,利用气相色谱仪测试了其纯度,并讨论了催化剂种类、用量、物料物质的量比、反应温度和反应时间等影响因素,确定了该反应的最佳条件。该方法收率高、能耗小、成本低,符合"原子经济性",易于实现工业化。
2-Methyl-allyl alcohol as the key initiator of polyether polycarboxylate superplasticizer was always synthesized by direct hydrolysis or two-step method of esterification and hydrolysis in tradition. This work introduces a one-pot method in which the two reactions of esterification and hydrolysis were accomplished in one cave,the yield can be over 90%,and the product was confirmed by the nuclear magnetic resonance(1H and13CNMR),IR and mass spectrometry( LRMS),its purity was checked by GC up to 98%; the optimization of conditions to synthesis 2-methyl-allyl alcohol was discussed by the catalyst and its amount,molar ratio of reagents,the time,the temperature and other factors. The method was very readily available and the operation was convenient,so it is potential to further applied in industrial production.