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Bwiti
(PVC-Analog Taste-Tester)
12-26-01 06:01
No 250484
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Quenching Grignard - Holy Shit!
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What's up?! A bear in my dreams said, "I reacted a methoxyphenyl Grignard with another interesting chemical and the reaction was hot enough to burn me when I placed my hand on the side of the jar. Good sign! The huge pickle jar was allowed to sit for about 20 hours, then it was time for quenching. I added a bunch of ammonia, water and a little ammonium chloride to it. It immediately got hot, then I had to bring it down to my basement, because it started to boil! I used excess Mg in my Grignard, so is that the reason for it being at a pissed off, violent boil? Can all this heat ruin my legal analogue? The bastard's been boiling for about 20 minutes now! I put a ceramic pot under it that's designed for ovens just in case the jar breaks. It just makes me nervous when I can't control a reaction. I thought about dumping all of it into a 10 gallon bucket and overwhelming it with water, but I'm worried that the solvents in the reaction mixture will dissolve the plastic. Help! <br><hr> Love my country. Fear my government.
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PrimoPyro<br>
<i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br>
<span title="Posting date">12-26-01 06:04</span><br>
<span title="Link to this post by using the markup [250485]">No 250485</span><br>
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<title>Re: Quenching Grignard - Holy Shit!
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Have you tried putting it inside dry ice/acetone bath?<br><br>That will suck a LOT of energy out of that reaction, especially if its a small container. It should stop the boiling, and may even make the reaction stop altogether!<br><br>Hell, just try a normal ice bath first and see what happens!<br><br> PrimoPyro<br><hr><font color="blue"><i>Vivent Longtemps la Ruche!</i></font color="blue">
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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">12-26-01 06:09</span><br>
<span title="Link to this post by using the markup [250486]">No 250486</span><br>
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<title>Re: Quenching Grignard - Holy Shit!
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No dry ice, but I do have some acetone..I would put it in an ice bath, but if the jar broke, it would spill everwhere.. I have to find a large pail. Peace!<br><hr> Love my country. Fear my government.
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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">12-26-01 06:24</span><br>
<span title="Link to this post by using the markup [250489]">No 250489</span><br>
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<b title="The subject of this post">Re: Quenching Grignard - Holy Shit!</b>
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I put on my oven mitts and put the jar into a mop bucket, then I added very cold water. I was gonna go up to the 7-11 and buy a bag of ice, but the cold water is working well by itself. I'm surprised the jar didn't crack. I'm using a ceramic plate as a cover for the jar. I opened it for a second, and all I could see was boiling grey matter. A little chem/water vapor hit me in the face when I opened it, and now I'm feeling a little altered! <br> When the chems are finished reacting, I need to separate the non-polar toluene, product, ether from the water and slop. Usually, I sprinkle sodium chloride into it until two distinct layers form, but I have a problem, because the salt I have is fucking iodized. How can I remove this shit from the salt? I'll just use TFSE to find other ways to bust up emulsions. <br>Peace and happy cooking!<img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"><br><hr> Love my country. Fear my government.
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PrimoPyro<br>
<i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br>
<span title="Posting date">12-26-01 16:32</span><br>
<span title="Link to this post by using the markup [250558]">No 250558</span><br>
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<b title="The subject of this post">Re: Quenching Grignard - Holy Shit!</b>
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Go buy non-iodized salt from the grocery store, and while you're there, pick up a ten lb bag of ice.<br><br>Both kinds of salt cost the same $2.25, and they are in the exact sae spot in the store. Some people cannot eat iodized salt, so straight NaCl is so common.<br><br> PrimoPyro<br><hr><font color="blue"><i>Vivent Longtemps la Ruche!</i></font color="blue">
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<font color="#ff0000">Osmium</font><br>
<i>(<span title="The user's title at the time of posting">Stoni's sexual toy</span>)</i><br>
<span title="Posting date">12-26-01 20:39</span><br>
<span title="Link to this post by using the markup [250584]">No 250584</span><br>
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<b title="The subject of this post">Re: Quenching Grignard - Holy Shit!</b>
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Arrrgh!<br>Iodized salt contains about 0.003% KIO3! What the fuck is the problem?!? Just use it dammit!
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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">12-26-01 22:04</span><br>
<span title="Link to this post by using the markup [250597]">No 250597</span><br>
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<b title="The subject of this post">Re: Quenching Grignard - Holy Shit!</b>
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"0.003%"<br><br> That's all? Thanks!<img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"><br><hr> Love my country. Fear my government.
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PolytheneSam<br>
<i>(<span title="The user's title at the time of posting">Master Searcher</span>)</i><br>
<span title="Posting date">12-27-01 00:36</span><br>
<span title="Link to this post by using the markup [250627]">No 250627</span><br>
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<b title="The subject of this post">Re: Quenching Grignard - Holy Shit!</b>
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When I was doing Grignard reactions in school (college) we were told to use a bucket of ice water to cool the reaction flask if needed. I found I needed ice with some Grignards at home, too. Ice always worked with the reactions I did (phenyl magnesium bromide and benzyl magnesium chloride).<br><hr>http://www.geocities.com/dritte123/PSPF.<wbr>html
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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">12-28-01 01:43</span><br>
<span title="Link to this post by using the markup [250842]">No 250842</span><br>
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<b title="The subject of this post">Re: Quenching Grignard - Holy Shit!</b>
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My product was ruined, but at least I've mastered the initiation of Grignards. <br><hr> Love my country. Fear my government.
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