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TheCopperMan
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Benzyl chlorides main effect should be a massive amount of tears in your eyes. If you smell it, you should also tear up almost immediately. If not
then it's something else. Have worked with it before and that was the first and last time. Need a full face mask to just be near it, and even then it
can hydrolyze with sweat on your skin and cause burns which was also experienced. The stuff is vicious.
[Edited on 23-6-2014 by TheCopperMan]
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pepsimax
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Is benzyl chloride soluble in xylene? According to wiki it shouldn't be, where as this stuff is. I poured some in and the gloops quickly dissolved in
it when swirled around. does anyone know the density of 4-chlorophenethylamine? Perhaps this is actually my free base oil and it's heavier than water
and extremely stinky.
The xylene was separated and washed with sat NaOH then brine and dried with MgSO4. This was diluted a bit with acetone and 10% H2SO4 with IPA was
dropped in and 13.4g of a sulphate salt was collected. that appears to be my yeild of this unknown compound!
[Edited on 23-6-2014 by pepsimax]
Ugh, I give up, apparently it is a dark solid.
[Edited on 23-6-2014 by pepsimax]
[Edited on 23-6-2014 by pepsimax]
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TheCopperMan
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Did you separate the other product from the steam distillate first, before you re-extracted it again with the Xylene? Or did you extract the entire
water distillate only once with everything in it, then add the sulfate to get the salt? (in which case it'd be a mixture of unknown stuff, and
phenetylamine)
[Edited on 23-6-2014 by TheCopperMan]
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pepsimax
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This was the gloopy stuff separated from the water distillate then put in fresh water to see if it sank again - it did, then dissolved in xylene. The
water from the steam pull didn't seem to have anything in it, i'm not sure what the stuff floating on it was, it didn't salt out to anything. I could
make the steam pull basic and try another solvent extraction, see what turns up
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TheCopperMan
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Hm, did you check the PH of the steam distillate?
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Crypto
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I tried to reduce nitromethane with Al/Cu today. I mixed 20ml of nitromethane with 50ml of IPA and 5ml of water. 1 gram of CuCl2 was dissolved in the
mixture and 5 grams of pretty thick aluminum ribbon was dumped in. The reaction started after a minute and it was really slow. It took a faster pace
after some heating was applied. Still, it was far from being vigorous. After about three hours no more action was observed. A lot of unreacted
aluminum was still present. Unfortunately I could not smell any methylamine during or after the reaction.
Maybe I should try again with a proton donor present in the mix?
Or maybe I just could not smell it and should basify, separate the aluminum sludge, add acid and try to isolate the salt, to determine if the reaction
occurred?
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pepsimax
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I didn't check the pH, too late now though as it has all been binned. I"ve found some aluminum swarf but it's pretty difficult to clean up. Washing in
caustic solution seems the best way.
Crypto, try with foil and preheat your solution and that should help. I've run this twice with ipa and got zero yield both times, no idea why but it
doesn't seem to work for me. Try ethanol maybe?
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ChemicalCowboy84
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What about mixing a little gallium with the aluminum foil plus using the CuCl2
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Burner
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If you use the gallium you do not need the CuCl2.
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ChemicalCowboy84
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So you think it would make the reaction run away ? I was just hypothesize that made it could help kick start the reaction with out the heating like a
regular al/hg reaction ? I believe we have something great here
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ChemicalCowboy84
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Also which CuCl2 should be used the anhydrous or dihydrate ?
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pepsimax
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Have you got any experience with this? I've tried all sorts of attempts with gallium and never got anything whether it be gallium salts or alloys.
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pepsimax
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Doesn't matter you'll dissolve it in water anyway
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TheCopperMan
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Working on some gallium experiments now actually.
Gallium is awesome in that it allows complete control of reaction, because the amalgam is made beforehand and then added gradually into the reaction
at a pace that you prefer.
The problem is, it's expensive, not all of it can be recycled (some dissolves), it's a pain in the ass to clean up the gallium post-reaction, and if
you touch the amalgam, drop it on the floor or etc, it's a pain to remove the stains it leaves.
[Edited on 29-6-2014 by TheCopperMan]
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Burner
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Quote: Originally posted by pepsimax  |
Have you got any experience with this? I've tried all sorts of attempts with gallium and never got anything whether it be gallium salts or alloys.
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I have used gallium in place of mercury (mole for mole) and the reactions proceed quite similarly. I have not been able to recover the gallium
easily, making this an expensive route for reductions.
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Burner
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| Quote: Originally posted by TheCopperMan | Working on some gallium experiments now actually.
Gallium is awesome in that it allows complete control of reaction, because the amalgam is made beforehand and then added gradually into the reaction
at a pace that you prefer.
The problem is, it's expensive, not all of it can be recycled (some dissolves), it's a pain in the ass to clean up the gallium post-reaction, and if
you touch the amalgam, drop it on the floor or etc, it's a pain to remove the stains it leaves.
[Edited on 29-6-2014 by TheCopperMan] |
I see someone else has explored this approach with similar results.
I do not recommend it, except for the learning experience, in which case it is excellent.
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TheCopperMan
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How much Ga did you use in place of mercury? Usually less than a gram mercury salt is used. Did you add it as a gallium salt or prepare amalgam
beforehand?
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pepsimax
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Another run....
5g substrate, 75ml reagent EtOH, 4.5g Al (half strips like first post, half of the strips rolled into ball, 600mg copper chloride heated to 50c in a
500ml flask. Flask was dropped in cold water whilst stirring full throttle. Al dissolved after 20mins, temp rose to 73 and dropped slowly to 40 when
the heat was turned on for gentle reflux. No nasty surprises this time. Just steaming it out now.
Gallium - are you using a salt? I made some gallium nitrate and that did nothing to foil when dropped in an aqueous solution of it, gallium chloride
didn't do much either but I suspect I made that wrong (just dissolved the nitrate in hcl and evaporated)
[Edited on 29-6-2014 by pepsimax]
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Burner
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| Quote: Originally posted by TheCopperMan | | How much Ga did you use in place of mercury? Usually less than a gram mercury salt is used. Did you add it as a gallium salt or prepare amalgam
beforehand? |
I used the gallium metal and prepared the aluminum amalgam using some aluminum shot that I had. I then let it sit overnight before I used it. Quite
simple really.
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Burner
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| Quote: Originally posted by pepsimax | Gallium - are you using a salt? I made some gallium nitrate and that did nothing to foil when dropped in an aqueous solution of it, gallium chloride
didn't do much either but I suspect I made that wrong (just dissolved the nitrate in hcl and evaporated)
[Edited on 29-6-2014 by pepsimax] |
I used the metal, not the salt.
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polsaer
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So, nobody have tried it on nitropropenes?
And why it working in EtOH, but not in IPA?
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Scr0t
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Probably some kind of solubility issue. I experienced something similar when attempting to reductively aminate cyclohexanone with aqueous NH3 and a
Zn-Ni couple. Best yields were with EtOH but were horrible with IPA.
My own attempts to get GaCl3 to react with Al foil failed but then I read a reference (maybe from these boards) that applied an electrostatic
potential to get a Ga salt to alloy.
[Edited on 2-7-2014 by Scr0t]
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pepsimax
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Been thinking, would this system run much smoother on nitrostyrene if the carbon carbon double bond was reduced with na borohydride first? Or is this
essential and I've missed this!
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TheCopperMan
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NaBH4 was never used, so it should perform without it.
BTW what was the result of the steam distillation? If you check the PH of the distillate, it should be basic indicating amine. You can then add acid
and evaporate the water to get the salt. Did you try this?
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crystal
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TheCopperMan, any attempts with gallium salts already? Gallium metal has been used before, and definitely works. As for the stains and recovery, I
recommend using dilute HCl. It makes gallium form blobs that are easy to separate.
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