节点文献
1,4-二氧杂螺[4.5]癸烷-8-酮的回收与提纯
Recycling and purification of 1,4-dioxaspirodecan-8-one
【摘要】 在生产液晶中间体4-羟基-4-(2,3-二氟-4-正丁氧基)苯基环己酮的废液中含有10%~30%的1,4-二氧杂螺[4.5]癸烷-8-酮,采用亚硫酸氢钠盐析法得到磺酸盐与有机物分离,然后还原得到1,4-二氧杂螺[4.5]癸烷-8-酮粗品,再经过重结晶得到合格的目的产品,GC含量>99.5%,回收率>80%。并对产品进行了GC-MSS,DCS,IR,1H NMR的确认。
【Abstract】 In the production of liquid crystal intermediates 4-hydroxy-4-(2,3-difluoro-4-n-butoxy) phenyl cyclohexanone liquid containing 10%~30% of 1,4-dioxaspirodecan-8-one,by using sodium bisulfite salting-out method with organic acid salt with organic separation,then 1,4-dioxaspirodecan-8-one was obtained.After crystallization of qualified products,content of target product.GC is over 99.5%.Recovery is over 80% and the products were characterized by GC-MSS,IR,1H NMR.
【关键词】 1,4-二氧杂螺[4.5]癸烷-8-酮;
单保护;
合成;
提纯;
【Key words】 1,4-dioxaspirodecan-8-one; monoprotection; synthesis; purification;
【Key words】 1,4-dioxaspirodecan-8-one; monoprotection; synthesis; purification;
【基金】 西安市重点技术创新项目
- 【文献出处】 应用化工 ,Applied Chemical Industry , 编辑部邮箱 ,2009年09期
- 【分类号】TQ25
- 【被引频次】1
- 【下载频次】85