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Harmonia
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| Joined: 04 Jul 2005 |
| Posts: 19 |
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613.02 Points
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Question regarding Al/Hg reduction of nitrostyrenes
Thu Jul 07, 2005 12:56 am |
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Procedure quoted from page on Rhodium's site:
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#1: The original procedure by Hyperlab Bee #1.
Into a 3 liter kitchen jar.....yes, exactly  .
So... into a 3 liter kitchen jar there’s placed:
- 75 mmoles of any nitrostyrene or phenylnitropropene (that should bee ~20 g) [Note 1]
- 200 mls GAA
- 300 mls IPA
- 100 mls water
- 0.75-1.3 g Hg(NO3)2 [Note 2]
Lastly, 40 g of kitchen Al foil is dumped into the soup.
The suspension is incubated for 30-40 mins after which it assumes black color and starts heating up.
At this moment SWIM simply takes the whole shebang and shakes it violently until the full dissolution of the nitro. At this point the mixture is usually vigorously boiling and is so hot that it can't bee held with bare hands.
From that moment the reaction proceeds for 5-10 mins, leaving a grey aluminous sludge as the result. The sludge is immediately dissolved in 300 g KOH in 800 mls water (which makes the mixture again boil so violently that the jar's bottom once fell off - after that we switched to using plastic canisters). Surprisingly, this treatment seems to not harm the product at all
The result is a two-phase mixture, the upper layer being the desired amine in IPA.
The procedure has been tested multiple times on the nitroalkenes corresponding to TMA-2, TMA-6 and 2C-H. It always gave yields not less than 70%. [Note 3]
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This looks like a very hazardous process.
Wouldn't it produce extreme heat, volcanoes etc? Or is it possible to go through with the reduction by adding all nitrostyrene, solvent, mercury salt and aluminium at once in a jar and just shake it, then take the lid off as long as you use a large container (I was thinking of a plastic can)?
Otherwise, is it preferrable to add nitrostyrene in solution to amalgamated aluminium, or aluminium to the nitrostyrene (in portions)?
(Obviously russian people are crazy.  ) |
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mk-1
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| Joined: 20 Feb 2005 |
| Posts: 86 |
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2841.38 Points
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re: Question regarding Al/Hg reduction of nitrostyrenes
Thu Jul 07, 2005 1:19 am |
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the way swim would suggest is this :
first preamalgamate all of ur Al. swim likes to make it the Al foil into rings, so when it is in solution it doesnt all go to the botoom but build up on each other.
Anyway, pre calculate how much Al u need, and amalgamate that,.
then in a differnt flask, dissolve all ur styrene in GAA and IPA, and add the pre amalgamated Al in small portions, allowing each portion to react fully. This way u keep the volcanoes to a minimum, and it just sounds better to swim |
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Harmonia
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| Joined: 04 Jul 2005 |
| Posts: 19 |
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613.02 Points
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re: Question regarding Al/Hg reduction of nitrostyrenes
Thu Jul 07, 2005 1:22 am |
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Thanks for your reply.
Sounds like a good idea, safetyminded.
But will I need external heating to keep the reactiong going? |
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mk-1
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| Joined: 20 Feb 2005 |
| Posts: 86 |
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2841.38 Points
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re: Question regarding Al/Hg reduction of nitrostyrenes
Thu Jul 07, 2005 2:22 am |
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slight heat may be needed. ud need to play it out and see how it goes. sometimes heat is needed, and sometimes it doesnt.
as the reaction is EXOthermic, once its started, its started, but since swim is doing it in small portions, and waits for the exo to end each time, heat might be neede. just play it as it goes... |
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