摘要
研究了以四氢呋喃为溶剂、格氏试剂合成法合成三正丁基膦的方法,对合成条件进行了优化,对合成产物进行了分析鉴定。结果表明:在镁、溴代正丁烷和三氯化磷的摩尔配比为1.05∶1.0∶0.27,格氏试剂制备的温度控制为回流温度,烷基化的温度控制在-3～0℃,反应时间分别为1.0、2.0h,三正丁基膦的收率最高,以溴代正丁烷计收率为53.1%。经折光和NMR分析确证为目标产品,GC归一化法分析质量分数为96.7%。
The synthesis of tri(n-butyl)phosphine in THF was introduced and synthetic conditions were optimilized. When THF was solvent, n(Mg)∶n(C_4H_9Br)∶n(PCl_3)is 1.05∶1.0∶0.27, temperature of Grignard reagent's synthesis is in reflux, temperature of alkylation is -3～0 ℃, reaction time is 1～2.0 h , yield of tri(n-butyl)phosphine in n-butyl bromide is 53.1%. The product was analyzed by RI,^(1)H-NMR,^(31)P-NMR and GC.
出处
《精细化工中间体》
CAS
2004年第6期39-41,共3页
Fine Chemical Intermediates
