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机构地区:[1]上海应用技术学院化学工程系,上海200235
出 处:《上海应用技术学院学报(自然科学版)》2005年第4期262-266,共5页Journal of Shanghai Institute of Technology: Natural Science
基 金:上海市科委重点攻关项目(034319254)
摘 要:以4-苯氧基苯酚,环氧丙烷为原料合成1-(4-苯氧基苯氧基)-2-丙醇,考察了物料比、反应时间、反应温度等因素对其收率的影响,得到最佳工艺条件。n(4-苯氧基苯酚):n(环氧丙烷):n(氢氧化钾)=1:3.0:0.3,反应温度40℃,反应时间3.5h,1-(4-苯氧基苯氧基)-2-丙醇收率最高达93.7%。以液相色谱法,采用LiChrospher 100 RP-18柱、甲醇+水为流动相、紫外检测器、外标法对1-(4-苯氧基苯氧基)-2-丙醇进行了高效液相色谱分析研究。方法标准偏差0.20%,变异系数0.23%,回收率在99.57%~100.52%之间。1- (4 - phenoxyphenoxy) propyl- 2 -ol was prepared from 4 - phenoxyphenol, and 1,2 - epoxypropane. The effect of reaction temperature, reaction time, dosage of 1,2 - epoxypropane and potassi- um hydrate on 1 - (4 - phenoxyphenoxy) propyl - 2 - ol were investigated. Optimized condition obtained were: n (4 - phenoxyphenol) : n (1,2 - epoxypropane) : n (potassium hydrate) = 1:3.0:0.3, temperature:40℃, reaction time: 3.5hrs. The yield of 1 - (4 - phenoxyphenoxy) propyl - 2 - ol can reach 93. 7%. HPLC method was developed for the determination of 1 - (4 - phenoxyphenoxy) propyl - 2 - ol on column LiChrospher 100 RP - 18. The mobile phase was methanol - water (73 + 27), and samples were detected by UV spectrometry at 230 nm. The recovery was 99.57% -100.52%. The product was characterized by IR, 1H NMR.
关 键 词:1-(4-苯氧基苯氧基)-2-丙醇 合成 分析 液相色谱
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