节点文献
2-氯-1,3,2-二氧磷杂环戊烷的合成
Synthesis of 2-Chloro-1,3,2-dioxaphospholane
【摘要】 合成了重要的有机中间体2 氯 1,3,2 二氧磷杂环戊烷.利用正交设计方法研究了反应温度、原料摩尔比、乙二醇滴加时间对反应收率的影响.实验结果表明:三氯化磷与乙二醇的最佳摩尔比为1.1∶1、最佳反应温度为4~6℃、加料时间为60~80min时,收率最高达到84.8%,远高于文献的报道(<70%).用元素分析和1HNMR表征了产物结构.
【Abstract】 Synthesized the useful organic intermediate 2-chloro-1,3,2-dioxaphospholane. Influences of reaction temperature, raw material molar ratio and dropwise time on the yield were studied with orthogonal plan method. The experimental results showed that the molar ratio of phosphorus trichloride to ethylene glycol, reaction temperature and the dropwise time were 1.1:1, 4~6 ℃ and 60~80 min, respectively. The best yield 84.8% is much higher than that of reported in literature. The structure of the product was characterized by elemental analysis and ()~1H NMR analysis.
【Key words】 dioxaphospholane; synthesis; orthogonal plan method; organic intermediate;
- 【文献出处】 化学研究 ,Chemical Researches , 编辑部邮箱 ,2004年03期
- 【分类号】O627.51
- 【被引频次】3
- 【下载频次】413