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阳明sir金虫 (正式写手)
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[求助]
氯化钯如何才能溶于乙腈
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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！！ |
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木虫 (正式写手)
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【答案】应助回帖
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阳明sir: 金币+20, 博学EPI+1, ★★★很有帮助, 谢了 2015-09-13 10:47:32
阳明sir: 金币+20, 博学EPI+1, ★★★很有帮助, 谢了 2015-09-13 10:47:32
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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 |
2楼2015-09-12 17:43:13
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木虫 (正式写手)
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阳明sir: 金币+10, ★★★很有帮助, 多谢 2015-09-13 10:47:46
阳明sir: 金币+10, ★★★很有帮助, 多谢 2015-09-13 10:47:46
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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 类似的 |
3楼2015-09-12 17:44:59