| 第 34 卷第 6 期 |  | Vol. 34 No. 6 | | 2004 年 12 月 | Dec 2004 |
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所屬欄目：其它
三正丁基膦的合成和表征 |
| 張驥紅; 陳峰; 陳雙飛(江蘇省化工研究所有限公司; 江蘇南京) |
| 摘 要：研究了以四氫呋喃為溶劑、格氏試劑合成法合成三正丁基膦的方法,對合成條件進(jìn)行了優(yōu)化,對合成產(chǎn)物進(jìn)行了分析鑒定。結果表明:在鎂、溴代正丁烷和三氯化磷的摩爾配比為1.05∶1.0∶0.27,格氏試劑制備的溫度控制為回流溫度,烷基化的溫度控制在-3～0℃,反應時(shí)間分別為1.0、2.0h,三正丁基膦的收率最高,以溴代正丁烷計收率為53.1%。經(jīng)折光和NMR分析確證為目標產(chǎn)品,GC歸一化法分析質(zhì)量分數為96.7%。 |
| 關(guān)鍵詞：三正丁基膦; 四氫呋喃; 溴代正丁烷; 合成 |
| 中圖分類(lèi)號：O627.51 文獻標識碼：A 文章編號：1009-9212(2004)06-0039-03 |
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| Synthesis and Identification of Tri(N-butyl)phosphine |
| ZHANG Ji-hong; CHEN Feng; CHEN Shuang-fei （Jiangsu Institute of Chemical Technology Co.Ltd.; Nanjing 210024; China） |
| Abstract：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. |
| Key words：tri（n-butyl）phosphine; THF; n-butyl bromide; synthesis |
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收稿日期：2004-08-19
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