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Author: Subject: 2,5-dimethoxyphenyl-2-nitropropene synthesis - 89.3% yield
Dextrose
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[*] posted on 18-12-2008 at 21:10


Quote:
Originally posted by Isomeric_Fred
I spoke to niobium, who said that EDDA is ethylenediamine diacetic acid salt.
Dextrose, i highly doubt a 75minutes reflux will yield well, niobium says it does not work well, and produces a red product, which once cleaned does give the yellowish 2,5-dmp2np but at lowered yields.
the Me.Am.Ac cat is good for other stuff, but less good for this one. Perhaps a shorter reflux period can yield well, or no reflux at all.


I must admit that i was wrong.
I did this condensation a couple of years ago with 200'ish of the aldehyde.
Got a yield of 90+% after a terrible clean-up, where i found out that MeOH is THE solvent to rxtl this nitrostyrene in.

I didn't do my calculations right, and just added up the catalyst (Me-acetate) from previous notes (duh!), and the product suddently crashed out after not more than 15 minutes, and i immediatly removed the condenser, and cooled the RB under cool running water.
(Yes, not more than 75 degrees celsuis, using a water bath and heavy stirring!)

Though i remember that there were a lot of impurities, that only the MeOH could remove - but still, the product was bright orange, and a recently Al/Hg-reduction of the 3 year (or so) old nitrostyrene, let to that i saw that it's supposed to be bright banana-yellow. (I was bored)

I'm sorry 'bout the bitching! - Anyway the Al/Hg worked out to my surprise (crap yield but what the fuck...) - i'll clean up the leftover nitrostyrene as soon as i get hold of some MeOH... no rush though.

Actually i hate the Al/Hg... talking about enviromental "harm reduction" in high yields in this topic, it is really a toxic pain in the ass! :(

And last, i did a variety of condensations back then, and another one with the same aldehyde and catalyst (way too much!), caused 50g or so to polymerize in just about 15 minutes also.

I didn't use the salt, but 40% methanolic MeNH2 and GAA.

Dex

[Edited on 19-12-2008 by Dextrose]
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brew
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[*] posted on 19-12-2008 at 01:56


The argument, that we should be able to discuss this chemistry, albeit leading to the possibility of this said chemistry being used to manafacture illegal compounds. and what a shame it would be, to have to deny such discussions etc, etc, Well the Ist sentence pretty well sets the stage of how this thread appears, dont you think, Well swim thinks so. Wave the fucking flag or what. Thats how it appears when you first read it, albeit from 2006 to now. It really annoys the hell out of me. Good chemistry, and the use of slang/ swim, etc, and then a defensive attitude when this is somewhat pointed out, it degrades it to just another meth dribble.

[Edited on 19-12-2008 by brew]
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stoichiometric_steve
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[*] posted on 19-12-2008 at 10:12


brew, what the fuck?



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brew
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[*] posted on 19-12-2008 at 15:55


WTF? I suppose I could cut and paste, but really cannot be bothered.
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DJF90
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[*] posted on 19-12-2008 at 16:39


brew has a valid point. Do you think that when Albert Hofmann first synthesised LSD he wrote in his lab book "swim made some LSD today"? Of course he didn't! Because he was a chemist, not a meth cook. I believe for interesting chemistry like this to be discussed, it should be discussed as chemistry, with the exclusion of terms like swim.

Such terms are in place to "decieve" others of your true intentions (you aren't fooling anyone!), and as chemists, our intentions *should* be honest (as we are only interested in the chemistry!). It does not matter that you made 2,5-dimethoxyphenyl-2-nitropropene, so long as you don't intend on finding an unsavoury use for it.
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Dextrose
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[*] posted on 19-12-2008 at 17:41


I don't get this... Are someone being flamed here, or did brew just had a bad day?

Where i am residing, none in this topic is illegal to practice in real life.

And... I'm not SWIMming anymore, and you shouldn't be either, since brew and DJF90 has a point about this.
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DJF90
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[*] posted on 19-12-2008 at 18:02


I don't think anyone is being flamed, I just think that swimming is pointless and a term employed by those trying to decieve others of their true intentions. If drug manufacture is "your thing", this isnt the place to discuss it, and as swim is a term associated with cooks, using it when describing a procedure (eg synthesis of precursors such as the one this thread is about) only causes (due) suspicion by others.

EDIT: This is fairly interesting chemistry, so can we please talk about it as chemists?

[Edited on 20-12-2008 by DJF90]
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Dextrose
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[*] posted on 19-12-2008 at 18:49


Yeah, science instead of point-less discussions.

Anyhow, i will point out that if you read "2,5-dimethoxyphenyl-2-nitropropene" and associates it with drug-chemistry - that's your fucking dirty mind, just like a pedophile would think of sex if he sees a 6-year old girl... Extreme comparison, i know, but i think you get my point.

I agree with stoichiometric_steve about the enviromental aspect in high yields - something i've never really given a thougt about... I would like to see some topics about "Eco-chemistry" :)

And BTW, i just realized that all the time i've been talking about the nitroSTYRENE, not the nitropropene... sorry for bringing in the confusion.

No blaming,
Dex!

[Edited on 20-12-2008 by Dextrose]
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DJF90
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[*] posted on 19-12-2008 at 19:39


What associates this thread with drug chemistry is the swimming on the first page, nothing to do with my mind. High yeilds are great, I agree, but tweaking a reaction to get a small % increase isn't going to benefit the environment much on this scale. If you are worried about making alot of waste then work on a smaller scale (Woelen is a good example of a chemist who works in an environmentally sound way - I'm sure there are others here but he is the first that comes to my mind).

And if you are accusing me of having a "dirty mind" because I see a thread about a precursor that involves swiming then I am very much guilty.
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Dextrose
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[*] posted on 19-12-2008 at 20:35


Like i wrote, no blaming, and no acusing - it wasn't directed at you, but at whoever might be reading this thread.
I'm sorry that it seems like it, it is merely a reply, but i hope you'll survive.

I've been swimming a lot, but drowned - and we ain't saints - or what? :P

[Edited on 20-12-2008 by Dextrose]
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brew
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[*] posted on 20-12-2008 at 14:45


I just read this, and wanted to clarify something. OUt of respect for the marjority of people who are into chemistry for the sake of chemistry, I wouldn't call myself swim. It not only redlights me, but it redlights this forum and I dare say many people want to be associated with this forum and for it not to necessarily infer that they are really cooks called swim. I am not against that chemistry or that particular compound as such, but when I see it written, and in particular for the type of compound it was referring to, and in this particular forum, I am going to react.

I really have no more to discuss on this matter, I wasn't flaming no -one in particular, Usually I dont say squat, but when I saw it , I reacted.
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[*] posted on 22-12-2008 at 08:58


Deleted the last three posts of this useless flame war.
"Swiming" is not allowed on this forum anyway, so I see no point in this discussion. The only reason why the original post of this thread contains the word "swim", or variants of it, is because it was posted before the ban.
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brew
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[*] posted on 22-12-2008 at 18:39


Okay, but I thought it was current as from 2008, and as I read it, after all thats been said on the matter etc, and to do with this particular compound etc, I reacted. I meant nothing personal to noone.
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tom_servo
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[*] posted on 23-12-2008 at 06:42


Quote:
Originally posted by enima
Yea, it works better >95% yields

I was under the impression that nitromethane would cause this reaction to not work at all or to give smaller yields.
Have you seen this first hand?
If so what ratios were used?

Never mind i thought you were talking about 3,4-methylenedioxyphenyl-2-nitropropene from piperonal

[Edited on 23-12-2008 by tom_servo]
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