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wangbaowk

新虫 (初入文坛)

应助: 0 (幼儿园)
金币: 27
红花: 1
帖子: 19
在线: 27.1小时
虫号: 1382949
注册: 2011-08-29
专业: 无机化工

[求助] 关于二价钌配位物的制备已有1人参与

大伙帮帮忙吧，我现在在做一个二价钌的催化剂，具体是双-(二甲基烯丙基）环辛-1,5-二烯钌，是1,5-环辛二烯二氯化钌和格氏试剂2-甲基烯丙基氯化镁制备得到的，我按照文献上的步骤，将两者反应的生成物，通过硅藻土，乙醚萃取，中性氧化铝过滤，蒸干等，最后也得到了文献所说的黑色残渣，文献上说加入甲醇会有固体析出，可是我做了很多次，第一次有固体析出，第二次也有，但是固体和第一次不同，还有几次是加入甲醇之后没有固体出来，等过一段时间才有稍许固体出来，请教一下这个是什么原理？？文献还说用甲醇-石油醚重结晶，可是甲醇和石油醚并不互溶，怎么重结晶啊，英文原文在下面：
This material was prepared using minor modiﬁcations to a literature procedure [2]. 2-Methylallylmagnesium chloride was found to be poorly soluble in Et2O and
therefore THF was used as the solvent. The Grignardreagent (2 M, 6 ml, 12 mmol; prepared from Mg and 3-chloro-2-methylpropene in THF) was added to a
suspension of [RuCl2(cod)]x (0.28 g, 1.0 mmol Ru) in Et2O (10 ml):THF (15 ml) and the mixture stirred at 20°C for 10 min. The excess Grignard reagent was
precipitated from solution by adding Et2O and the suspension was ﬁltered through Celite. The ﬁltrate was hydrolyzed in ice-water and the mixture extracted with
Et2O(220 ml). The organic layer was dried over MgSO4, concentrated, ﬁltered through a short column of neutral alumina (55 cm) and evaporated to dry-
ness. Reprecipitation from a mixture of MeOH and petroleum ether gave pure 1

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