Bwiti
(PVC-Analog Taste-Tester)
12-26-01 06:01
No 250484
      Quenching Grignard - Holy Shit!  Bookmark   

  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! 

  Love my country. Fear my government.
 
 
 
 
    PrimoPyro
(Hive Addict)
12-26-01 06:04
No 250485
      Re: Quenching Grignard - Holy Shit!  Bookmark   

Have you tried putting it inside dry ice/acetone bath?

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!

Hell, just try a normal ice bath first and see what happens!

                                                 PrimoPyro

Vivent Longtemps la Ruche!
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
12-26-01 06:09
No 250486
      Re: Quenching Grignard - Holy Shit!  Bookmark   

  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!

  Love my country. Fear my government.
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
12-26-01 06:24
No 250489
      Re: Quenching Grignard - Holy Shit!  Bookmark   

  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!
  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.
Peace and happy cooking!cool

  Love my country. Fear my government.
 
 
 
 
    PrimoPyro
(Hive Addict)
12-26-01 16:32
No 250558
      Re: Quenching Grignard - Holy Shit!  Bookmark   

Go buy non-iodized salt from the grocery store, and while you're there, pick up a ten lb bag of ice.

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.

                                                  PrimoPyro

Vivent Longtemps la Ruche!
 
 
 
 
    Osmium
(Stoni's sexual toy)
12-26-01 20:39
No 250584
      Re: Quenching Grignard - Holy Shit!  Bookmark   

Arrrgh!
Iodized salt contains about 0.003% KIO3! What the fuck is the problem?!? Just use it dammit!
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
12-26-01 22:04
No 250597
      Re: Quenching Grignard - Holy Shit!  Bookmark   

"0.003%"

  That's all? Thanks!cool

  Love my country. Fear my government.
 
 
 
 
    PolytheneSam
(Master Searcher)
12-27-01 00:36
No 250627
      Re: Quenching Grignard - Holy Shit!  Bookmark   

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).

http://www.geocities.com/dritte123/PSPF.html
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
12-28-01 01:43
No 250842
      Re: Quenching Grignard - Holy Shit!  Bookmark   

  My product was ruined, but at least I've mastered the initiation of Grignards.

  Love my country. Fear my government.