Chlorohydridotris(triphenylphosphine)ruthenium(II)
Chlorohydridotris(triphenylphosphine)ruthenium(II)
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氯氢化三(三苯基膦)钌(II)
DOI：
10.1002/9780470132449.ch26
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发表时间：
2007
期刊：
影响因子：
--
通讯作者：
G. Wilkinson
中科院分区：
文献类型：
--
作者：
R. A. Schunn;E. Wonchoba;G. Wilkinson
注意事项。氢气是一种高度易燃易爆气体，反应应在通风橱中进行。整个过程在干燥的氮气气氛中进行。500毫升，三颈烧瓶配备有磁力搅拌器和Glass Col加热套。烧瓶的一个颈部装有进气管，该进气管将突出到150 ml的表面下方。并连接到干燥氢源上。烧瓶的第二颈装有顶部有T形管的高效回流冷凝器，T形管的一侧连接到干燥氮气源，另一侧连接到硅油起泡器。用氮气彻底吹扫烧瓶，并装入9.5g。（0.0078摩尔）的[{（CsH 5）3 P）4 R-C12]，22.4g。（0.024摩尔）三乙胺和150 ml.脱氧甲苯将烧瓶的第三颈塞住，搅拌混合物并加热至回流，同时使H2的缓慢流通过棕色混合物。将氢气通入水溶液1小时，在此期间颜色从棕色变为紫色，并形成紫色结晶固体。停止氢气流，并将混合物在冰水中冷却1小时以确保完全结晶。然后将混合物在惰性气氛中过滤（见注释），用5个50 ml洗涤紫色结晶固体。部分脱氧乙醇和两个25-ml.部分脱氧甲苯。将固体在25 ″/0.01 p下干燥1小时，得到7.23 g。(90%）的[{（C6 H5）3 P）3RuHCl]。C6 H5 CH 3 mp分解> 150”。以这种方式获得的产物对于大多数用途来说是足够纯的，但是可以从热甲苯（~ 1g/l）中重结晶。160毫升）。和Calcd。对于C1H5&1P3Ru的分析计算：C，72.2; H，5.4; Cl，3.5; P，9.1。实测值：C，72.0; H，5.6; Cl，3.7; P，9.4。
Procedure rn Caution. Hydrogen is a highly jlammable, explosive gas and the reaction should be conducted in an eficient fume hood. The entire procedure is performed in a dry nitrogen atmosphere. A 500-ml., three-necked flask is equipped with a magnetic stirrer and Glass Col heating mantle. One neck of the flask is fitted with a gas inlet tube which will protrude beneath the surface of the 150 ml. of solvent to be used and is attached to a source of dry hydrogen. The second neck of the flask is fitted with an efficient reflux condenser topped with a T tube, one side of which is attached to a source of dry nitrogen and the other to a silicon oil bubbler. The flask is purged thoroughly with nitrogen and charged with 9.5 g.(0.0078 mole) of [{(CsHs) 3P) 4R~ C12], 2 2.4 g.(0.024 mole) of triethylamine, and 150 ml. of deoxygenated toluene. The third neck of the flask is stoppered, and the mixture is stirred and heated to reflux while a slow stream of Hz is passed through the brown mixture. Hydrogen is passed through the refluxing solution for one hour during which the color changes from brown to purple, and a purple, crystalline solid is formed. The hydrogen flow is stopped, and the mixture is cooled in ice-water for one hour to ensure complete crystallization. The mixture is then filtered in an inert atmosphere (see Note) and the purple, crystalline solid is washed with five 50-ml. portions of deoxygenated ethanol and two 25-ml. portions of deoxygenated toluene. The solid is dried at 25"/0.01 p for one hour to give 7.23 g.(90%) of [{(C6H5) 3P) 3RuHCI]. C6H5CH3 mp decomp.> 150". The product obtained in this manner is sufficiently pure for most uses but may be recrystallized from hot toluene (-1 g./160 ml.). And Calcd. for CslH5&1P3Ru: C, 72.2; H, 5.4; C1, 3.5; P, 9.1. Found: C, 72.0; H, 5.6; C1, 3.7; P, 9.4.