I usually start the addition when I don't see any shine left on the surface of the Al. No the temperature change won't effect the reaction.
Re: Short Question Thread 2.0
« Reply #360 on: April 11, 2013, 02:57:39 AM »
Topic: Short Question Thread 2.0 (Read 5709 times)
fractal
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bjuice
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Re: Short Question Thread 2.0
« Reply #361 on: April 11, 2013, 03:36:41 AM »
Thanks again fractal. One more question.
On the low-yielding Al/Hg I was talking about a few posts back: after the reaction had stirred overnight I basified with KOH rather than the often quoted NaOH. I don't see why it would make a substantial difference, but, could this possibly be reason for my low yield?
On the low-yielding Al/Hg I was talking about a few posts back: after the reaction had stirred overnight I basified with KOH rather than the often quoted NaOH. I don't see why it would make a substantial difference, but, could this possibly be reason for my low yield?
fractal
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Re: Short Question Thread 2.0
« Reply #362 on: April 11, 2013, 04:13:41 AM »
Nope, KOH works just as well. It's possible that your oxidation didn't run to completion. Did you use a vigreux column when distilling? Absolutely positive you had only one product? What oxidation did you use to synthesize your ketone?
bjuice
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Re: Short Question Thread 2.0
« Reply #363 on: April 11, 2013, 04:38:47 AM »
No, didn't use a vigruex but what came over looked just like I've seen it described. Clean yellow color with a neon tinge. It had a unique consistency -- sort of a high surface tension. The word that comes to mind is "globular", yet liquidy. Smelled sweet and "spicy".
Oxidation was buffered peracetic a la Chromic, followed by the HCl Pinacol. Overall yield from iso to mdp2p was around 40%, which isn't great but not terrible. After distilling the ketone there was a lot of leftover brown goop/tar in the bottom, which I'm thinking may have been due to some leftover HCl in the mix as a result of poor workup (back-extracted water with DCM, but didn't wash the back-extract like I should have). Hard to quantify, but it seems like yields were great in the peracetic, and dropped a lot with the Pinacol.
You know, I just realized what the issue probably was: poor stirring. The Al/Hg was 45g mdp2p in a 2 liter RBF, and while the 2.5" stirbar was going the entire time, only the bottom layer was actually stirring. There was a lot of goop down at the bottom preventing the stirring motion from propagating upward to the entire reaction mixture. If it makes any difference, the reaction was left stirring on low heat overnight.
I'm thinking a flat bottomed flask and a larger stir bar would be more appropriate. An overhead stirrer just isn't in my budget, and I've heard plenty of success with a stir bar.
Oxidation was buffered peracetic a la Chromic, followed by the HCl Pinacol. Overall yield from iso to mdp2p was around 40%, which isn't great but not terrible. After distilling the ketone there was a lot of leftover brown goop/tar in the bottom, which I'm thinking may have been due to some leftover HCl in the mix as a result of poor workup (back-extracted water with DCM, but didn't wash the back-extract like I should have). Hard to quantify, but it seems like yields were great in the peracetic, and dropped a lot with the Pinacol.
You know, I just realized what the issue probably was: poor stirring. The Al/Hg was 45g mdp2p in a 2 liter RBF, and while the 2.5" stirbar was going the entire time, only the bottom layer was actually stirring. There was a lot of goop down at the bottom preventing the stirring motion from propagating upward to the entire reaction mixture. If it makes any difference, the reaction was left stirring on low heat overnight.
I'm thinking a flat bottomed flask and a larger stir bar would be more appropriate. An overhead stirrer just isn't in my budget, and I've heard plenty of success with a stir bar.
RoidRage
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Re: Short Question Thread 2.0
« Reply #364 on: April 11, 2013, 02:27:38 PM »
When initiating an Al/Hg in a 2 liters flask, I usually help the stir bar by shaking the flask from time to time until the whole reaction mixture is able to be stirred by the stir bar.
Flight
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Re: Short Question Thread 2.0
« Reply #365 on: April 12, 2013, 05:50:30 AM »
Hello,
I did a boiling point test of about 50ml, because I didn't have a little test tube, and thankfully it boiled right on the dot 232C. By doing this test at atmospheric pressure did I do damage to the sample? I UTFSE, but didn't see an exact answer.
Thanks,
Flight
I did a boiling point test of about 50ml, because I didn't have a little test tube, and thankfully it boiled right on the dot 232C. By doing this test at atmospheric pressure did I do damage to the sample? I UTFSE, but didn't see an exact answer.
Thanks,
Flight
Sneak
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Re: Short Question Thread 2.0
« Reply #366 on: April 12, 2013, 08:22:26 AM »
You may have potentially scorched some of it at that temp at atmospheric. I have seen it mentioned a few times. You also may not have. 
organics decompose above 300*c I believe.
Get a cheap asspirate-or.
organics decompose above 300*c I believe. Get a cheap asspirate-or.
Flight
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Re: Short Question Thread 2.0
« Reply #367 on: April 12, 2013, 01:56:06 PM »
A vacuum pump is available, but just wanted to have a clear understanding of the BP. Hopefully it wasn't scorch, as soon as it reached temp it was removed from the hotplate.
Thanks for your help
Thanks for your help
bjuice
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Re: Short Question Thread 2.0
« Reply #368 on: April 13, 2013, 12:56:40 AM »
In case anyone cares to know, the final yield after recrystallization and acetone rinse was 9.6g MDMA.HCl from 45g MDP2P, a 17% yield. Not terrible and I have some ideas on how to improve the next run. Thanks for the help guys!
Tsjanga
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Re: Short Question Thread 2.0
« Reply #369 on: April 13, 2013, 09:02:08 AM »
If we use sesamol on a Reimer-Tiemann formylation and work from there would that be any good?
I hate the OH on this substance it is even stronger bonded than on ephedrine...
I hate the OH on this substance it is even stronger bonded than on ephedrine...
Flight
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Re: Short Question Thread 2.0
« Reply #370 on: April 14, 2013, 06:07:40 PM »
"Buffered Performic write-up/pictorial for newbees"
"Using a 2L flask, this is the most iso you can convert to keep control of the reaction IMHO."
300 grams iso
91 grams Sodium Bicarbonate(Arm n hammer )
800 ml DCM
279 grams H2O2 35%
461 grams Formic acid 88%
If only a 1 liter flask is available can these numbers simply be cut if half.
Thank you, all of you have been so helpful.
"Using a 2L flask, this is the most iso you can convert to keep control of the reaction IMHO."
300 grams iso
91 grams Sodium Bicarbonate(Arm n hammer )
800 ml DCM
279 grams H2O2 35%
461 grams Formic acid 88%
If only a 1 liter flask is available can these numbers simply be cut if half.
Thank you, all of you have been so helpful.
RoidRage
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Re: Short Question Thread 2.0
« Reply #371 on: April 14, 2013, 07:53:45 PM »
"Buffered Performic write-up/pictorial for newbees"
"Using a 2L flask, this is the most iso you can convert to keep control of the reaction IMHO."
300 grams iso
91 grams Sodium Bicarbonate(Arm n hammer )
800 ml DCM
279 grams H2O2 35%
461 grams Formic acid 88%
If only a 1 liter flask is available can these numbers simply be cut if half.
Thank you, all of you have been so helpful.
Yes
no1uno
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Re: Short Question Thread 2.0
« Reply #372 on: April 15, 2013, 11:31:45 AM »
Naproxen - presumably it forms an amide, which on Hoffman degradation would give 6-OH-naphthyl-2-ethyl-1-amine(
). Now I'm thinking, if that were so, then hydrolysis of the amine would give the 6-methoxynaphthyl-2-acetone, which should be able to be cleaved to the 6-methoxyNaphthyl-2-carboxylic acid, the amide of which would give the 6-methoxynaphthyl-2-amine. If 6-Cl-2-aminotetralin is an active, rigid & non-psychotoxic analog of p-cl-amphetamine, presumably this would, on reduction, be a non-neurotoxic p-methoxy-amphetamine? Just musing, the structure is just begging for something to be done to it.
The names of the compounds would be naproxen amide, hoffman degradation to 6-methoxynaphthalene-2-ethyl-1-amine, hydrolysis to 6-methoxynaphthalene-2-ethanone, cleavage of the ketone would give 6-methoxy-2-napthoic acid and the amide from that would be 6-methoxy-2-naphthamide (prices for which start at US$32/2mg), so it has to be good for something. Lithium + NH3/EtNH2 reduces the wrong ring giving the 6-carboxytetralol, but that might be useful if the tetralol could be oxidized to the ketone and aminated giving 6-carboxy-2-aminotetralin.
). Now I'm thinking, if that were so, then hydrolysis of the amine would give the 6-methoxynaphthyl-2-acetone, which should be able to be cleaved to the 6-methoxyNaphthyl-2-carboxylic acid, the amide of which would give the 6-methoxynaphthyl-2-amine. If 6-Cl-2-aminotetralin is an active, rigid & non-psychotoxic analog of p-cl-amphetamine, presumably this would, on reduction, be a non-neurotoxic p-methoxy-amphetamine? Just musing, the structure is just begging for something to be done to it.The names of the compounds would be naproxen amide, hoffman degradation to 6-methoxynaphthalene-2-ethyl-1-amine, hydrolysis to 6-methoxynaphthalene-2-ethanone, cleavage of the ketone would give 6-methoxy-2-napthoic acid and the amide from that would be 6-methoxy-2-naphthamide (prices for which start at US$32/2mg), so it has to be good for something. Lithium + NH3/EtNH2 reduces the wrong ring giving the 6-carboxytetralol, but that might be useful if the tetralol could be oxidized to the ketone and aminated giving 6-carboxy-2-aminotetralin.
Naproxen.to.6.methoxy.2.amino.naphthalene.pdf
(10.45 kB - downloaded 4 times.)bosan
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Re: Short Question Thread 2.0
« Reply #373 on: April 15, 2013, 11:48:26 PM »
super noob question.
Lots of syths start with Isosaf, but the "fist time" ones (brightstar or methyl man) don't mention which step obtains isosaf.
erowid has some steps to obtain, but curious what the people here prefer to obtain the coveted isosaf?
anyone watched this one:
https://www.youtube.com/watch?v=KtY-y6KXS9s
Lots of syths start with Isosaf, but the "fist time" ones (brightstar or methyl man) don't mention which step obtains isosaf.
erowid has some steps to obtain, but curious what the people here prefer to obtain the coveted isosaf?
anyone watched this one:
https://www.youtube.com/watch?v=KtY-y6KXS9s
fractal
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Re: Short Question Thread 2.0
« Reply #374 on: April 16, 2013, 12:02:48 AM »
Brightstar doesn't mention an isosafrole synthesis because one isn't done. You don't need to when doing a Wacker oxidation. You do though when doing a Performic or peracetic oxidation if you want your carbonyl the right place. You should read what's going on instead of JUST write ups and things will make a lot more sense.
pbinteger
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Re: Short Question Thread 2.0
« Reply #375 on: April 16, 2013, 03:29:24 AM »
Amen Fractal -- one needs to know the basics to do any troubleshooting -- read up on thermodynamics, atomic physics -- learn at least SOME of the nomenclature for the functional groups you're working with.
GENERAL CHEMISTRY, Linus Pauling ISBN --486-65622-5 is a great primer
_Pbint_
GENERAL CHEMISTRY, Linus Pauling ISBN --486-65622-5 is a great primer
_Pbint_
Sneak
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Re: Short Question Thread 2.0
« Reply #376 on: April 16, 2013, 12:07:29 PM »
archive.org/details/CollegeChemistry
There's a copy.
Cheers pb! Looks a good en!
There's a copy.
Cheers pb! Looks a good en!
carbonated
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Re: Short Question Thread 2.0
« Reply #377 on: April 16, 2013, 01:52:44 PM »
A 56 year-old Chemistry book is the best option out there? I'm confused...
There are probably a lot more accurate and easier to understand options out there than that, imo. I'd start with the khanacademy.org Organic Chemistry videos and work your way up from there. Pirating a newish copy of an O Chem book shouldn't be a problem either.
I'm confused... There are probably a lot more accurate and easier to understand options out there than that, imo. I'd start with the khanacademy.org Organic Chemistry videos and work your way up from there. Pirating a newish copy of an O Chem book shouldn't be a problem either.
Sneak
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Re: Short Question Thread 2.0
« Reply #378 on: April 16, 2013, 03:14:52 PM »
Yes indeed upon closer inspection, that's rather old. I like it though, it's got that vintage feel to it.
I need a fucking laptop so I can use all these torrents. Android phones do not cut it when used to study chemistry...
Or am I about to be enlightened...?
I need a fucking laptop so I can use all these torrents. Android phones do not cut it when used to study chemistry...
Or am I about to be enlightened...?
Flight
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Re: Short Question Thread 2.0
« Reply #379 on: April 17, 2013, 05:20:13 PM »
Buffered Performic Route....
How does one calculate the amount of H2O2 to use? So instead of using 35% say only 29% is available. Also, is using 29% a good idea or should only 35% be used.
Thanks,
F
How does one calculate the amount of H2O2 to use? So instead of using 35% say only 29% is available. Also, is using 29% a good idea or should only 35% be used.
Thanks,
F