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Dr_Sister
(Hive Bee)
12-30-01 09:51
No 251356
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Work-up - DMSO Al/Hg
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for reasons she won't get into now, yer sistah thought dmso might be an appropriate solvent for a Al/Hg reduction she's been visualizing. However, being unfamiliar with that solvents properties, she is unsure how to work-it up. The rxn product is a molecule that is very heat intolerant, so stripping off the dmso under vac is not the 1st avenue she wants to explore. A previoous rxn's product was destroyed in an attempt to steam distill the hydroxylamine out of the dmso.(dumb, i know)<br><br>come on make yer sistah smile. help!<br><hr>7.10.01
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<font color="#FF0033">Rhodium</font><br>
<i>(<span title="The user's title at the time of posting">Chief Bee</span>)</i><br>
<span title="Posting date">12-30-01 11:34</span><br>
<span title="Link to this post by using the markup [251367]">No 251367</span><br>
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<title>Re: Work-up - DMSO Al/Hg
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I would dilute the DMSO with large amounts of water (3-5x the DMSO volume), and after basifying, extracting the solution with <b>many portions of DCM (if you are really serious, test each extraction with TLC for presence of your product, and when it is no longer visible, stop the extraction.
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Dr_Sister<br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">12-30-01 11:46</span><br>
<span title="Link to this post by using the markup [251370]">No 251370</span><br>
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<title>Re: Work-up - DMSO Al/Hg</b>
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<img src="../forum/images/icons_lightgrey/smile.gif" alt="smile" title="Smile" heigth="15" width="15"> thanks<br><hr>7.10.01
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hest<br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">01-02-02 07:39</span><br>
<span title="Link to this post by using the markup [251980]">No 251980</span><br>
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<b title="The subject of this post">Re: Work-up - DMSO Al/Hg</b>
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you might reduce the DMSO, happens with LiALH4. And dimethylsulphide is not a nice smell to produce
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Dr_Sister<br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">01-02-02 16:24</span><br>
<span title="Link to this post by using the markup [252062]">No 252062</span><br>
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<b title="The subject of this post">Re: Work-up - DMSO Al/Hg</b>
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that wouldn't be a pungent rotten vegetable smell would it?<br><hr>7.10.01
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<font color="#FF0033">Rhodium</font><br>
<i>(<span title="The user's title at the time of posting">Chief Bee</span>)</i><br>
<span title="Posting date">01-02-02 18:35</span><br>
<span title="Link to this post by using the markup [252094]">No 252094</span><br>
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<b title="The subject of this post">Re: Work-up - DMSO Al/Hg</b>
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That or worse.
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Dr_Sister<br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">01-02-02 20:41</span><br>
<span title="Link to this post by using the markup [252126]">No 252126</span><br>
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<b title="The subject of this post">What a joke!</b>
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<img src="../forum/images/icons_lightgrey/laugh.gif" alt="laugh" title="Laugh" heigth="15" width="15">LOL, this has got to go down as the 1st honest to goodeness fuck-up of 2002, it smells like hell, and with a BP of 38 its no wonder. The MSDS describes the odor as: STENCH hahahahah. I couldn't figure out what the fuck was causing that smell, was thinking more along the lines of decomposed product. I guess that pretty much sums it up for DMSO Al/Hg. The whole idea was to avoid the stink of thf, hahahahhah what a joke. the hotter the rxn got the more it stunk to christ, almost as bad as methylamine just different.<br><br>yer sister has tears streaming down her face<img src="../forum/images/icons_lightgrey/laugh.gif" alt="laugh" title="Laugh" heigth="15" width="15"><br><hr>7.10.01
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