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Bwiti
(PVC-Analog Taste-Tester)
12-13-01 04:35
No 246963
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Drying Ether With NaOH
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I was told that the use of baked Mg-sulfate on ether won't render it dry enough for a Grignard, so I'll use NaOH instead. This red devil lye has to be bone-dry before I add it to the ether..Do I need to bake it in the oven at 318C (melting point), or would that be over-doing it? After drying the ether, could I just decant it from the lye and use it in the Grignard, or should I distill it? Thanks and peace!<img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"><br><hr> Split a piece of wood and I am there. Lift a stone and you will find me.
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b159510<br>
<i>(<span title="The user's title at the time of posting">Professional Student</span>)</i><br>
<span title="Posting date">12-13-01 07:17</span><br>
<span title="Link to this post by using the markup [247005]">No 247005</span><br>
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<title>Re: Drying Ether With NaOH
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NaOH to dry ether? not<br><br><font color="blue">Do I need to bake it in the oven at 318C (melting point), or would that be over-doing it</font color="blue"><br><br>that would be funny to watch<br><br>[EDIT] < insert constructive comment here--> I don't think your friend knows what s/he is talking about.<br>Hmm. Well it looks like it was your idea to use NaOH, not your friends. So it looks like you don't know what your talking about. Please give my apologies to your friend.<br> <hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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terbium<br>
<i>(<span title="The user's title at the time of posting">Old P2P Cook</span>)</i><br>
<span title="Posting date">12-13-01 07:48</span><br>
<span title="Link to this post by using the markup [247015]">No 247015</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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Neither magnesium sulfate or sodium hydroxide will get ether as dry as is traditionally considered necessary for use it a Grignard.<br><br>Recently (the past few months) I think that there was a post about using microwave heating to kick-start a Grignard (or was it ultrasound - geez, my memory is failing me). Perhaps this would help start a Grignard with ether that is wetter than is normally considered acceptable.<br><br>A traditional way to dry ether for a Grignard would be to distill it from metallic sodium (seems like metallic lithium from a battery could be substituted) and a little quinone (benzoquinone/hydroquinone). A person I once worked for liked to use potassium metal/TiCL4 instead of the sodium/quinone.
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terbium<br>
<i>(<span title="The user's title at the time of posting">Old P2P Cook</span>)</i><br>
<span title="Posting date">12-13-01 07:58</span><br>
<span title="Link to this post by using the markup [247021]">No 247021</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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Yep, my memory is failing fast. I guess it must be ultrasound that I had read about. See the thread starting with <span title="Jump to this post"><a href="../DUMMY">Post 174625</a> <i>(uemura: "Grignard Startup", Methods Discourse)</i></span> . And, in this thread, lugh claims that caustic soda (crude NaOH such as Red Devil) will dry ether enough for a Grignard <span title="Jump to this post"><a href="../DUMMY">Post 174765</a> <i>(lugh: "Re: Grignard Startup", Methods Discourse)</i></span> .
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b159510<br>
<i>(<span title="The user's title at the time of posting">Professional Student</span>)</i><br>
<span title="Posting date">12-13-01 08:18</span><br>
<span title="Link to this post by using the markup [247033]">No 247033</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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So, add NaOH to your wet ether to dry it?<br>Don't be shocked when your reaction fails.<br>If it works I'll be the shocked one.<br><br><hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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<font color="#ff0000">lugh</font><br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">12-13-01 12:44</span><br>
<span title="Link to this post by using the markup [247093]">No 247093</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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<blockquote title="Quoted text"><hr><p>If it works I'll be the shocked one.<p><hr></blockquote><p><br><br>Better make sure you're not grounded, wouldn't want to see you get crispy fried <img src="../forum/images/icons_lightgrey/smile.gif" alt="smile" title="Smile" heigth="15" width="15"> See <i>Science</i> <b>87</b> 171 (1938) for details. This procedure takes two weeks to work, that's why it never became popular <img src="../forum/images/icons_lightgrey/smile.gif" alt="smile" title="Smile" heigth="15" width="15"><br><br>
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Bwiti<br>
<i>(<span title="The user's title at the time of posting">PVC-Analog Taste-Tester</span>)</i><br>
<span title="Posting date">12-13-01 18:27</span><br>
<span title="Link to this post by using the markup [247142]">No 247142</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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"See Science 87 171 (1938) for details."<br><br> The university I live near is more geared towards engineering, so I can't find articles like the above there. Could someone please scan it, post it on poppies.org, then link it to here? I say this because The Hive only accepts images to post if they already have a url. Thanks!<br> Thanks for the info Terbium! My ultrasonicator worked when I had shitty ether, while I was working with bromobenzene..Maybe Grignards with methoxybromobenzene are harder to initiate? I'm starting to think that the glass of my flask is too thick for the ultrasonic waves to sufficiently penetrate? Maybe I should initiate it in something with thinner glass like a test tube or even a light bulb, then dump it into the bulk? The next time I dick with a Grignard, I'll be sure to obtain some potassium, but for now I'll attempt it again using NaOH. I guess I'll dry it in the oven at 220*F? <br><br>"So it looks like you don't know what your talking about."<br><br> b159510: Were you always an asshole, or did something happen to you as a child to make you this way. It always pisses me off when some trouser-stain such as yourself replies, cuts others down to bring himself up. When you were molested by your uncle, did you feel ashamed that you liked it? You are a waste of humanity, you're an abortion that got away and your comments aren't welcome here, so why don't you go back to seducing 8 year-olds on yahoo chat. <br> <img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"><br><hr> Split a piece of wood and I am there. Lift a stone and you will find me.
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b159510<br>
<i>(<span title="The user's title at the time of posting">Professional Student</span>)</i><br>
<span title="Posting date">12-13-01 20:11</span><br>
<span title="Link to this post by using the markup [247175]">No 247175</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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ahahahahaha.....funny.<br><br>i wasn't putting you down to lift myself up. what would i do that for?<br><br>i was just laughing at the procedure you came up with.<br><br>drying NaOH in an oven? i assume this is not some hi-tech oven. who has ever heard of such a thing? no way you could 'dry' NaOH in an oven. i'll let you figure out why.<br><br>there are established ways of drying ether - using NaOH is not one of them. i could go into details, but i won't.<br><br>you are correct though, i never was going to tell you how to dry ether, so i shouldn't have said anything.<br><br>i apologize to you for responding to your post in a less than helpful manner. i've been trying not to do that.<br><br>-sorry-<br><hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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timsong<br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">12-13-01 20:57</span><br>
<span title="Link to this post by using the markup [247186]">No 247186</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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Not everyone has the best reagents for various processes. This is one of the things the hive is about, discussing alternative methods, using/trying one thing instead of another.<br>If you don't ask/try, you'll never no !<br>Ridicule is not helpfull. I have seen many bees eat there own hats over methods they considered wrong in the past.
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b159510<br>
<i>(<span title="The user's title at the time of posting">Professional Student</span>)</i><br>
<span title="Posting date">12-13-01 21:51</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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<font color="blue"> have seen many bees eat there own hats over methods they considered wrong in the past. </font color="blue">...<br><br>true. but if you divide that number by the number of posts<br>proposing absurd procedures and multiply by 100 you would be<br>looking at about 5%. <br><br>i would ask - what part of this do you find credible-<br>drying ether with NaOH? drying NaOH in your oven?<br><br>perhaps it is not necessary to titrate a NaOH solution<br>anymore. just put the NaOH in an oven then weigh it out.<br>shit, that would save a lot of people a lot of time eh?<br><br>whatever - i know i shouldn't have said anything if i wasn't<br>going to give a better way. and since i'm not, goodbye<br><br><br><hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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<font color="#ff0000">lugh</font><br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">12-13-01 22:11</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b><br>
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No reason to get excited, there are many useful techniques of organic chemistry not known to the masses, discussing them is the true purpose of this site <img src="../forum/images/icons_lightgrey/smile.gif" alt="smile" title="Smile" heigth="15" width="15"> The procedure is ancient and very simple, Mr. Bruce writes to add one pound of technical grade sodium hydroxide to three liters of USP grade ether, and wait two weeks <img src="../forum/images/icons_lightgrey/smile.gif" alt="smile" title="Smile" heigth="15" width="15"> When compared with commercial anhydrous ether by Forbes and Coolidge, in JACS <b>41</b> 150 (1919). using strongly alkaline potassium permagnate, found the reaction time for USP ether to be three seconds, commercial absolute ether twelve seconds and sodium hydroxide dried ether twenty seconds, so this procedure produces a drier ether than sodium wire <img src="../forum/images/icons_lightgrey/laugh.gif" alt="laugh" title="Laugh" heigth="15" width="15">
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Bwiti<br>
<i>(<span title="The user's title at the time of posting">PVC-Analog Taste-Tester</span>)</i><br>
<span title="Posting date">12-13-01 22:29</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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2 weeks? I'm in no rush. Sounds like a plan.<br><br>"strongly alkaline potassium permagnate"<br><br> Have plenty of permanganate. How would I go about making it strongly alkaline?<br><hr> Split a piece of wood and I am there. Lift a stone and you will find me.
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b159510<br>
<i>(<span title="The user's title at the time of posting">Professional Student</span>)</i><br>
<span title="Posting date">12-13-01 22:31</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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<font color="blue">so this procedure produces a drier ether than sodium wire </font color="blue">....yes, that is surprising to me. a mix of potassium and sodium with bubbling nitrogen is how i have distilled dry ether. took a little and added a few drops of bzphenone to check for oxides. i have also used ether for the gringard that had simply been stirred overnight with anydrous mag sulfate, and it worked fine. go figure. <hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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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">12-13-01 22:34</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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1. MgSO4 dryet ether is dry enough for Grignard.<br>2. NaOH is a fine drying regent.<br>3. Usual it the purity of the Mg in the Grignard there is the problem.<br>4. Adding 1% Dibromoethane to the bromide before adding to the Mg turnings helps alot.<br>
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<font color="#ff0000">lugh</font><br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">12-13-01 22:49</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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<blockquote title="Quoted text"><hr><p>Have plenty of permanganate. How would I go about making it strongly alkaline?<p><hr></blockquote><p><br><br>Generally one uses a base, but why do you need to duplicate the test procedure?
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Bwiti<br>
<i>(<span title="The user's title at the time of posting">PVC-Analog Taste-Tester</span>)</i><br>
<span title="Posting date">12-13-01 23:06</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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"but why do you need to duplicate the test procedure?"<br><br> Just for shits and giggles.<br><br>"Adding 1% Dibromoethane to the bromide before adding to the Mg turnings helps alot."<br><br> Never tried that. In the past, I've found it to be helpful to grind the Mg powder with anhydrous Mg-chloride. I got the idea from a patent at <a href="http://gb.espacenet.com/" target="_blank" title="Jump to this external site">http://gb.espacenet.com/</a> , but I can't remember the fucking #. Wonder if Na or K - iodide would work as a good catalyst?<br><br><hr> Split a piece of wood and I am there. Lift a stone and you will find me.
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b159510<br>
<i>(<span title="The user's title at the time of posting">Professional Student</span>)</i><br>
<span title="Posting date">12-14-01 00:04</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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wouldn't simply dissolving KMnO<sub>4</sub> is minimal<br>water make a strongly basic solution? (in the form of KOH)<br><hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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Lino<br>
<i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br>
<span title="Posting date">12-14-01 04:28</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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Bwiti, I thought I told you about drying stuff for grignards previously<img src="../forum/images/icons_lightgrey/smile.gif" alt="smile" title="Smile" heigth="15" width="15">. Buy Et20 with 0.2 % or less H2O. Dry over CaCl, Na, (not recommended) or 4a mol seives (recomended).<br><br>Glassware dried in oven for 1-2 hrs @ 200º ish. Or better, on the hotplate like what SWIL used to do. It really did work.<br><br>To initiate Grignard crush Mg 'curlies' (previously dried in flask on hotplate for 30 mins)w/ a glass rod or similar. It starts to get a bit cloudy around the 'crushed' Mg area then goes off like fookin hell. have a water bath and wet towel ready. Addition should be fast enough to keep the bastard going or it goes out.<br><br>Beest wishes<br><hr>Linoleum: the 13th element! Now available at all good DIY stores… & Walmart.
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<font color="#FF0033">Lilienthal</font><br>
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<span title="Posting date">12-15-01 21:04</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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b159510: The benzophenone is simply a water indicator. It forms a dark blue solution if the mixture is totally anhydrous (due to Na reduction to it's coloured radical which would be degraded by water).
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b159510<br>
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<span title="Posting date">12-16-01 00:13</span><br>
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<b title="The subject of this post">Re: Drying Ether With NaOH</b>
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lilienthal - that is interesting. i'll look into that because i thought i was testing for free oxygen, and some oxides. i didn't think it was a test for water. molecular oxygen is a diradical, so maybe thats why it works. <hr><font color="blue"><i>Back to the Primitive</i></font color="blue">
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