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氯化钯如何才能溶于乙腈

作者 阳明sir
来源: 小木虫 100 2 举报帖子
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最近的实验需要将氯化钯溶于乙腈,但是太贵了不敢贸然下手,不知道氯化钯是否可以直接溶于乙腈,或者如何操作能够使其溶于乙腈,
望不吝赐教!!!!定重谢!! 返回小木虫查看更多

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    [Pd(CH3CN)2Cl2]. The procedure is adapted from that already
    described for the corresponding benzonitrile complexes.57 Palladium
    chloride was suspended in acetonitrile (120 ml CH3CN per
    gram of PdCl2) and refluxed for 2 h allowing PdCl2 to essentially
    dissolve completely. The hot solution was filtered through
    filtering paper with the aid of a cannula to remove very small
    amounts of undissolved impurities. The solution was then cooled
    at 0 °C to promote [Pd(CH3CN)2Cl2] precipitation. The yellow
    solid was recovered by filtration with a Buchner. The remaining
    solution was then evaporated in vacuo to afford additional
    complex (quantitative yield). Calcd for C4H6N2Cl2Pd: C, 18.52;
    H, 2.33; N, 10.80%. Found: C, 18.78, H, 2.26; N, 10.72%. δH
    (CDCl3, RT, 300 MHz): 2,40 (s, CH3). The spectrum also shows
    a signal at 2.03 ppm indicating free acetonitrile. Aweak signal at
    2.39 ppm is also observable. IR (nujol): 2335, 2304 cm−1 (in
    accord with the literature58) IR (C2H4Cl2): 2337, 2306 cm−1.

    Dalton Trans., 2012,41, 3648-3658
    这是做氯化钯乙腈配合物的,他就是先把PdCl2放在乙腈里加热回流,让其溶解,然后降温析晶。所以前面溶解的部分可以参考,

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    Bis(acetonitrile)dichloropalladium(II), Pd(MeCN)2Cl2, was prepared from PdCl2 as described: PdCl2 (2.0 g,
    11.3 mmol) was suspended in dry MeCN (450 mL). The reaction mixture was heated to reflux for 3 hours under argon atmosphere. After cooling down to room temperature (23°C) the solvent was removed under reduced pressure. The remaining solid was dried under high vacuum and the title compound was received in quantitative yield (2.9 g) as an orange-yellow solid. The dried product can be used without further purification and was stored under argon in the dark。
    Org. Lett. 2015, 17, 2478−2481
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