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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
[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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