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DNA
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I think it would be nice actually to steam distill the freebase directly out of the reaction mixture, this prevents you from dealing with large
amounts of zinc salts and the whole reaction mixture crap.
After the steam distillation you will have your freebase very pure which also enhances the bromination.
And when it forms the carbonate then it does but actually it is not a problem if it does so, because before the bromination you will dissolve it in
glacial acetic acid anyway so if you have the carbonate salt or the HCl salt or the freebase it is all the same in the end of the day 
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smuv
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precipitate the zinc salts w/ oxalic acid, remove the zinc oxalate, then deal with them amine...
"Titanium tetrachloride…You sly temptress." --Walter Bishop
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gonzo
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2c-h distilling
hi. is it possible to distill 2c-h with an aspirator vacuum ? what is the boiling point of 2c-h ? Is an 100mmHg vacuum enough to distill it ?
thanx in advance
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DNA
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No it is not enough vacuum to distill 2C-H.
I don't know the boiling point by heart but you can look it up in pihkal.
Then with a nomograph you can calculate the boiling point at 100mmHg but probably the 2C-H will decompose at the temperature you will need at
100mmHg.
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gardenvariety
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Has anyone attempted to bubble HCl into the alcohol rather than using 31% in water? I'm wondering if you could get substantially more nitrostyrene
into a batch if the solvent wasn't half water.
Going to try this and compare in a few weeks but wondering if anyone else looked down that path.
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xwinorb
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I have never tried it. The yield is quite high already anyway.
My best 75 %, my worse 55 %.
The more significant factor I could relate to higher yields was the color ( I guess that means purity ) of the nitrostyrene.
When I used a more dull, brownish one, the yields were lower. When the nitrostyrene had a better, nice, bright orange color the yield was better.
It works.
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Bronstein
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I was thinking about using this procedure to reduce another nitrostyrene and I thought what smuv wrote about using oxalic acid seemed intreresting.
Quote: Originally posted by smuv  | | precipitate the zinc salts w/ oxalic acid, remove the zinc oxalate, then deal with them amine... |
But when I think more about it, to precipitate the 100g zinc used in this procedure you would need 192g oxalic acid (dihydrate). And oxalic acid
dissolves at ~14g/100ml water (according to wiki), so if you dissolved it before you added it you would need more than 1.3L of water. And this
reaction already has a quite large volume.
But perhaps you could add it dry directly to the reaction mixture?
Or perhaps it's not worth the extra trouble to use oxalic acid, I don't know...
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