How you will try to synth the Oxime?
Electro´S
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carl_nnabis
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Is your problem to source THF? Look out in european hardware stores, its used to glue pond foil together, but it is a mixture containing MEK, cyclohexanone, ethylacetat and other shit, but is composed usually 1/3 or 1/2 out of THF.
Remember to store your purified THF properly then, THF-peroxide is really scary stuff! A friend said to me if you ever notice crystals on your thf-can leave the place call the bomb squad and most important dont even look at the peroxide crystals they may see this as a provocation to explode!
Store your THF over sodium or add some stabilizer, BHT, ionone, some copper etc.
Remember to store your purified THF properly then, THF-peroxide is really scary stuff! A friend said to me if you ever notice crystals on your thf-can leave the place call the bomb squad and most important dont even look at the peroxide crystals they may see this as a provocation to explode!
Store your THF over sodium or add some stabilizer, BHT, ionone, some copper etc.
Electro´S
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WOW!!! THF Peroxides!?!?!?!
I think than Electrolysis would be a good option for the oxime.
I think than Electrolysis would be a good option for the oxime.
carl_nnabis
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They only become a problem after very long time storage without stabilizer! Like, two years or else.
The electroreduction seems like a good way to the amine as well, not only to the oxime?
Anyway, look into the attached document, i had a quick read through the hydroxylamine chapter, it starts at 6.3, and it seems methanol substitutes for THF, what implys you can use other polar aprotic solvent as well maybe. As long as they dissolve your educct good enough.
Polar aprotic solvents are but not limited to: methanol, acetonitrile, nitromethane, DMSO, DMF.
The electroreduction seems like a good way to the amine as well, not only to the oxime?
Anyway, look into the attached document, i had a quick read through the hydroxylamine chapter, it starts at 6.3, and it seems methanol substitutes for THF, what implys you can use other polar aprotic solvent as well maybe. As long as they dissolve your educct good enough.
Polar aprotic solvents are but not limited to: methanol, acetonitrile, nitromethane, DMSO, DMF.
Electro´S
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.......
carl_nnabis
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hey electro,
im not sure really if it works as you wish to brominating it. Better iodinate/brominate it straight, with iodine/bromine in glacial acetic acid with some catalytic red phosphorus added. This would be most convenient in my opinion. You can also esterify your norephedrine, with, maybe an o-acetyl group? Then CTH reduction using Pd/C or whatever is most well suited for you.
Oh, and yes, you probably have to reflux it. Dont own the needed equipment yet? Check ebay its really cheap if you are lucky, or pm me i know some cheap supplier here.
im not sure really if it works as you wish to brominating it. Better iodinate/brominate it straight, with iodine/bromine in glacial acetic acid with some catalytic red phosphorus added. This would be most convenient in my opinion. You can also esterify your norephedrine, with, maybe an o-acetyl group? Then CTH reduction using Pd/C or whatever is most well suited for you.
Oh, and yes, you probably have to reflux it. Dont own the needed equipment yet? Check ebay its really cheap if you are lucky, or pm me i know some cheap supplier here.
fishinabottle
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Quote
What you think about this route?Complete nonsense.
You have everything to go via P2NP in decent yields, do it.
Electro´S
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QuoteWhat you think about this route?Complete nonsense.
You have everything to go via P2NP in decent yields, do it.
Yes I know, but the decent yields is hard to get.
What would be your recommendation after P2NP???
At the moment, Tin Cl2·2H2O to oxime had been success. And after a little Al/Hg amalgam of the oxime a little yield is obtained, but the most clean and pure product i saw.
Zinc /activated with Hg (just because i can't find in vogel the famous obvious reference for old bees about activating zinc with HCl) with and without ammonium formate in methanol and in acetic acid.
BTW, any reference about the process for Tin Chloride regeneration in the Oxime formation???
I know than my question are a lot of times obvious for bees with experience or studies. But for self-taught beekeeping likes me is hard to understand what happend inside the flask when the stirrer is turned On. Anyways i am hard working reading all the pdf´s shared in this "Hive" and now i know more chemist than before...
Thanks all for Share your time and your knowledge.
carl_nnabis
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you have access to Hg and you are familiar with reduction of MDP2NP via the same route, so why dont you reduce it straight with this route?
Electro´S
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You are talking about Nitroalkenes Al/Hg???
The yields are so bad in all my attemps, and is impossible scale it up.
However Oxime Al/Hg look like more gentyl and the scale limit will be a little up than nitroalkene reduction.
And if Zinc/ammonium formate works... Is the faster reaction. But two attemps the yield was nothing.
I know than NaBH4 to the alkane would be the best option, and them a lot of doors are open but i have not access to it, and it is expensive like the hell.
The yields are so bad in all my attemps, and is impossible scale it up.
However Oxime Al/Hg look like more gentyl and the scale limit will be a little up than nitroalkene reduction.
And if Zinc/ammonium formate works... Is the faster reaction. But two attemps the yield was nothing.
I know than NaBH4 to the alkane would be the best option, and them a lot of doors are open but i have not access to it, and it is expensive like the hell.
Happyman
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Hey guys, I got my first vacuum pump up and running yesterday, the only problem is the gauge has no units! The gauge goes from 0-30 mystery units and I can draw a vacuum anywhere from 0-20 mystery units. Any guesses on what units this gauge uses?
lugh
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Quote
Hey guys, I got my first vacuum pump up and running yesterday, the only problem is the gauge has no units! The gauge goes from 0-30 mystery units and I can draw a vacuum anywhere from 0-20 mystery units. Any guesses on what units this gauge uses?
An old thread in which answers to such questions was posted:
https://the-collective.ws/forum/index.php?topic=22762.0
embezzler
- Subordinate Wasp
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It is most likely PSI or inches of Mercury. My money would be on the former.
gloves
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Question may be slightly off-topic, but I didn't find what I was looking for (if it still exists) and I thought it'd have been better to use this thread than creating something new for such a silly question.
I think there was a PDF about nicotine extraction hosted here, but am unable to find it. Does anybody have a mirrorlink?
Thank you
I think there was a PDF about nicotine extraction hosted here, but am unable to find it. Does anybody have a mirrorlink?
Thank you
POSEIDON
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Question may be slightly off-topic, but I didn't find what I was looking for (if it still exists) and I thought it'd have been better to use this thread than creating something new for such a silly question.
I think there was a PDF about nicotine extraction hosted here, but am unable to find it. Does anybody have a mirrorlink?
Thank you
look in this book page 190
http://babel.hathitrust.org/cgi/pt?id=mdp.39015069112228
Winston
- Larvae
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AFOAF showed me some so called white phosphorous. He had it in a plastic bag which was in a plastic bag etc etc. When looking at it, it looked waxy. I took a little bit out, and let it sit in a darkened space, and I could not see any blueish/greenish color, nor did it self ignite. I just did a very rough m.p and it was around 40deg celcius. Is there anything else I can do to be sure this is what it is claimed to be. I am not familiar with this element, and do not have access of my UNI equipment. I will try a flame test, but thought I could ask here, just in case there is a very simple test. MY hunch is its a salt, but why the low melting point if that is so, so i am not sure.
Winston
- Larvae
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Nah,.Ill just put it in test tube, add a little D.I. water, heat, and bubble in O2, if it doesn't ignite then its not WP Sorry folks, I was just being lazy, and looking for short cuts. Cheers.
Tsathoggua
- Autistic sociopath
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The smell would bee a decent indicator. WP has a fairly distinctive garlic-like odour. Doesn't take much to give off enough to recognize it (although remember that WP is highly toxic stuff......and sequelae from WP burns can last for some time after the actual wound heals. Got left with a severely weakened arm post accident with the stuff as a kid, took several weeks until I was able to write, or do anything requiring much grip strength or fine motor coordination.
Happyman
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If I can smell ether when distilling it under vacuum, what is the best way to look for leaks?
lugh
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Quote
If I can smell ether when distilling it under vacuum, what is the best way to look for leaks?
It's probably coming out the exhaust Oil pumps aren't generally used for distilling ether since it's so volatile