Author Topic: Short Questions Thread  (Read 10825 times)

Tungsten.

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Re: Short Questions Thread
« Reply #660 on: November 11, 2010, 12:31:36 AM »
I have a question about this use of Urushibara Nickel to reduce phenolnitropropene: http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/amph.urushibara.html Is this just a typo that it says that it is Urushibara Nickel instead of Raney Nickel (because he precipitates the nickel onto aluminum instead of zinc?), or am I getting the difference in the two confused?

Also, does anyone have a good way to extract the benzaldehyde from grocery store almond extract? Or can I make phenolnitropropene from it in its solution of "water, 32% alcohol, benzaldehyde"?

Thanks all. ;)
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lugh

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Re: Short Questions Thread
« Reply #661 on: November 11, 2010, 02:23:37 AM »
Ritter did exactly what he posted  ;) Clearly you need to do more studying about your interests as the information you seek has been available for a decade 8)
Chemistry is our Covalent Bond

Sedit

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Re: Short Questions Thread
« Reply #662 on: November 11, 2010, 06:47:00 AM »
What would be the simplest means to Methylate a Carbon carbon Pi bond? I have researched the use of Dimsyl ions followed with thermal decomposition to yeild the methylated product but this sounds as though it could get messy in some cases and I was woundering what others thought here. Would MeI and the likes accomplish this? Im having a hard time finding any answers because ironicly these g'damn drug forums and threads are clogging up google search engines when I try to find methylation information.
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Tungsten.

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Re: Short Questions Thread
« Reply #663 on: November 11, 2010, 11:41:28 AM »
Ritter did exactly what he posted  ;) Clearly you need to do more studying about your interests as the information you seek has been available for a decade 8)

Oh, you're right. I was just being dumb. I see what the difference between the two is now. ;)
-W

atara

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Re: Short Questions Thread
« Reply #664 on: November 11, 2010, 05:03:00 PM »
What would be the simplest means to Methylate a Carbon carbon Pi bond? I have researched the use of Dimsyl ions followed with thermal decomposition to yeild the methylated product but this sounds as though it could get messy in some cases and I was woundering what others thought here. Would MeI and the likes accomplish this? Im having a hard time finding any answers because ironicly these g'damn drug forums and threads are clogging up google search engines when I try to find methylation information.

Uh, please describe in more detail the reaction you wish to achieve!

Sedit

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Re: Short Questions Thread
« Reply #665 on: November 11, 2010, 05:29:58 PM »
I wish to saturate a double bound by placing a methyl across it mainly that of a nitrostyrene which complicates things a little bit more.
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Enkidu

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Re: Short Questions Thread
« Reply #666 on: November 11, 2010, 09:12:42 PM »
Check Comprehensive Organic Functional Group Transformations I and also II by Katritzky et al and  Comprehensive Organic Transformations. A guide to functional group preparations by Larock. I'm sure you'll find something.

Sedit

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Re: Short Questions Thread
« Reply #667 on: November 13, 2010, 04:02:27 AM »
You can't by any chance perhaps provide a link or an upload can you Enkidu? Im still having trouble finding information on methylating reagents for such a task although I did stumble across an interesting comment about someone using fresh MeOH+H2SO4 for the methylation of unsaturated fatty acids.
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Tungsten.

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Re: Short Questions Thread
« Reply #668 on: November 13, 2010, 06:17:07 AM »
-W

Enkidu

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Re: Short Questions Thread
« Reply #669 on: November 18, 2010, 07:09:09 AM »
I wish to saturate a double bound by placing a methyl across it mainly that of a nitrostyrene which complicates things a little bit more.
Did you ever find anything?

Sedit

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Re: Short Questions Thread
« Reply #670 on: November 18, 2010, 07:52:38 AM »
uggg no not completely.

But I have focused my searches on locating a methylating reagent to add to the alpha position of basic styrene. That should clear up some confusion by eliminating the worried of the attached nitro group.

Still its a shock how lacking the scientific communitys papers are on something as simple as placing a Me across a double bond theres next to no information on such a thing which I find odd. Iv been at it for over 2 weeks now and all methylation of Pi bonds seems focused on extending the chain.

BTW fun times ahead fellows I just eliminated the need for Al/Hg using something as simple as NiSO4/NaCl/CuSO4 and Al so lets move along with this styrene experiment so I can put it into a format all these stupid cooks can use.
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solidstone

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Re: Short Questions Thread
« Reply #671 on: November 22, 2010, 12:26:17 AM »
I was thinking you could take styrene, add a halogen to get the dihalide.  treat with NaOH or KOH to get the alkyne.  Use electrolysis to prepare some sodium metal, make sodium amide using the sodium and ammonia.  Create the Acetylide ion of styrene then treat with bromo methane (or another halomethane) to get the chain addition to the right length.  Then treat the phenyl pro-2-yne with acid and mercury acetate or something to give the enol to tautomerize to the ketone. giving a mixed product which should be mostly p2p from styrene (that theoretically could be rendered from pyrolosis of styrofoam).

It also looks like you can get away with doing this without the mercury acetate although sources say the conditions are much more vigorous due to an unstable vinylic carbocation or something along those lines.  If it worked without the mercury acetate this would be an even more feasible route.

Or are you trying to just add the N-methyl Sedit?
« Last Edit: November 22, 2010, 12:35:17 AM by solidstone »

solidstone

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Re: Short Questions Thread
« Reply #672 on: November 22, 2010, 12:51:32 AM »
Quick question.  I am looking at erowid.org/archive/rhodium/chemistry/ether2ester.hypochlorite.html#refs
I am wondering if the hypochlorites would be effective in converting the analogous secondary alcohol in codeine (analogous to cyclohexanol) into codeinone, and how I would go about testing I in fact made the ketone.  The quicker the solution the better.
gas evolution, precipitate, oil formation, difference in physical characteristics in general would be of much help to me here.
Thanks in advance.

Enkidu

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Re: Short Questions Thread
« Reply #673 on: November 22, 2010, 07:10:33 AM »
melting point, Codeinone having a melting point of 165-167°C

You really should run TLC

solidstone

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Re: Short Questions Thread
« Reply #674 on: November 22, 2010, 07:23:37 AM »
TLC against what?  codeine?  I need a reference, correct?  how will I tell if the epoxide is oxidized or the Nitrogen affected by the sodium hypochlorite.  I guess MP and TLC. 

Tungsten.

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Re: Short Questions Thread
« Reply #675 on: November 22, 2010, 01:37:51 PM »
TLC: hxxp://en.wikipedia.org/wiki/Thin_layer_chromatography
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Sedit

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Re: Short Questions Thread
« Reply #676 on: November 22, 2010, 07:00:46 PM »
You run a TLC from the start of the experiment, just a small dot on the plate then as the reaction progresses you put a couple more spots inbetween as the reaction proceeds. Develop these side by side and look for variations in the spots to see if anything new forms.
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Vesp

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Re: Short Questions Thread
« Reply #677 on: November 28, 2010, 07:40:56 AM »
Is Aesculetin, if readily available, a practical precursor to TMA-2?
http://en.wikipedia.org/wiki/Aesculetin
into...

It looks like it could hydrolyze into 2,4,5-trihydroxycinnamic acid - which has serious potential, assuming the ability to methoxylate and turn the acid into the aldehyde or something, right?

I am not to sure on how safe it would be to hydrolyse, especially with all the other OH groups - it would obviously be very prone to oxidation, but it does seem possible... any comments on such?

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Wizard X

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Re: Short Questions Thread
« Reply #678 on: November 28, 2010, 10:44:12 PM »


Synthesize the methylenedioxy ring first, then hydrolyse to ring open to 4,5-methylenedioxy-2-hydroxycinnamic acid.
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

Vesp

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Re: Short Questions Thread
« Reply #679 on: November 28, 2010, 11:47:57 PM »
Why would you want to do this?
I was thinking, if anything - methoxylate it first and than hydrolyse it.
Is there a reason the 4,5-methylenedioxy would be wanted? Seems like that would lead to more trouble..

and than the hydrolysis would just be to take the coumarin like substance and turn it into the 2-hydroxycinnamic acid with something like refluxing in a KOH solution?

Unless you are thinking of something like MMDA-2
« Last Edit: November 29, 2010, 12:35:34 AM by Vesp »
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