摘要
对(-)-α-蒎烯的氧化条件进行了详细的研究,以获得(+)-2,3-蒎烷二醇的高选择性制备方法。考察了氧化剂用量、反应温度、反应体系pH值、溶剂种类和用量、体系水量、反应时间等因素对(-)-α-蒎烯氧化反应的影响,并通过单因素试验确定了适宜的氧化条件,结果表明:氧化剂用量0.2 mol,溶解高锰酸钾的NaOH水溶液用量与原料α-蒎烯的比例为37∶1(mL∶g),将高锰酸钾溶解在pH值为13的氢氧化钠水溶液中,然后缓慢滴入系统。溶剂叔丁醇的用量为料液比1∶16(g∶mL),过氧化物抑制剂乙二醇用量1.44 mol,反应温度为40℃,反应时间为4 h。在最适条件下,产物(+)-2,3蒎烷二醇的平均选择性为90.1%(n=3)。采用GC-MS和1 H NMR对产物的结构进行了表征,确定合成了(+)-2,3-蒎烷二醇。
The detailed investigation of the oxidation conditions for(-)-α-pinene aimed at obtaining an environmentally highly selective synthesis method for(+)-2,3-pinanediol.This study explored the impact of various factors including the quantity of oxidant,reaction temperature,pH value of the reaction medium,solvent type and volume,system water content,and reaction duration,on the oxidation process of(-)-α-pinene.Through single factor experiments optimal oxidation conditions were established as follows:the oxidant dosage was 0.2 mol,the solvent-to-reactant ratio of potassium permanganate NaOH aqueous solution to raw materialα-pinene was 37∶1(mL∶g),potassium permanganate was dissolved in a sodium hydroxide solution with pH value of 13,and then slowly dripped to the reaction mixture,the solvent tert-butanol was used at a solid-liquid ratio of 1∶16(g∶mL),the dosage of the peroxide inhibitor ethylene glycol was 1.44 mol,the reaction was conducted at a controlled temperature of 40℃for a period of 4 h.Under the optimum conditions,the average selectivity of the praduct(+)-2,3-pinanediol was 90.1%(n=3).The synthesis of(+)-2,3-pinanediol was determined by the characterization of the products structure using GC-MS and 1 H NMR.
作者
秦顾天越
刘炜祺
杨益琴
徐徐
王忠龙
王石发
QIN Gutianyue;LIU Weiqi;YANG Yiqin;XU Xu;WANG Zhonglong;WANG Shifa(College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,China;College of Light Industry and Food,Nanjing Forestry University,Nanjing 210037,China)
出处
《林产化学与工业》
北大核心
2025年第4期139-144,共6页
Chemistry and Industry of Forest Products
基金
国家重点研发计划资助项目(2022YFD2200801)。
