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2-乙醇吡啶溶解于极性溶剂中,在高效加氢催化剂作用下及一定压力及温度下与氢气反应一定时间得到2-乙醇哌啶反应液。将制得的2-乙醇哌啶溶解于非极性溶剂中,控制反应温度,同时滴加氯甲酸仲丁酯,经酸洗、水洗处理后,脱溶得到羟哌酯粗品。将羟哌酯粗品在真空及高温条件下蒸馏得到羟哌酯成品。考察了各反应因素对两步反应的影响,确定了最佳合成工艺:2-乙醇吡啶在4MPa压力下,催化加氢反应10h得到2-乙醇哌啶,再在室温下滴加与其摩尔比为1∶1.3的氯甲酸仲丁酯反应1h。
2-ethanol pyridine dissolved in a polar solvent, under the effect of efficient hydrogenation catalyst and a certain pressure and temperature reaction with hydrogen gas to obtain 2-ethanol piperidine reaction solution. The prepared 2-ethanol piperidine is dissolved in a non-polar solvent, the reaction temperature is controlled, while sec-butyl chloroformate is added dropwise, the acid is washed and washed with water, and then the crude solution is obtained through desolvation. The crude product of piperidin in distilled under vacuum and high temperature to obtain the finished product of piperacol. The effects of reaction factors on the two-step reaction were investigated. The optimum synthesis conditions were determined: 2-ethanol-pyridine under 2MPa pressure, catalytic hydrogenation reaction for 10h to obtain 2-ethanol piperidine, and then at room temperature with the molar ratio of 1: 1.3 of sec-butyl chloroformate reaction 1h.