Successful [Large] RXN

[Organikum]

and did what perhaps nobody has done before - I read all the articles. And the more interesting ones not only once.

The ephedrine cleavage for determination of ephedrine content by the amount iodine used up in the procedure was done during the practical organic laboratory lessons at a german university. I will send you the text with reaction mechanism as soon I am able to upload stuff again. (in german of course)

If you were right on what you say on ayiridines and this Rhodium, than every halogenation of alcohols with phosphorus/iodine by I3 as described in VOGELs, the Gattermann and the ORGANIKUM (just to name a few) would have the same bad results. But they all speak of 90% to quantitative yields - probably a conspiracy I guess.

must go
ORG

[Rhodium]

If you were right on what you say on ayiridines and this Rhodium, than every halogenation of alcohols with phosphorus/iodine by I3 as described in VOGELs, the Gattermann and the ORGANIKUM (just to name a few) would have the same bad results. But they all speak of 90% to quantitative yields - probably a conspiracy I guess.

The halogenation of the benzylic alcohol to the corresponding iodide probably goes to completion relatively quickly. 

I am mostly talking about the further reduction of iodoephedrine to methamphetamine, which does not go to completion unless given time to do so. The aziridine formation is a intramolecular cyclization of iodoephedrine (favored by high temperatures), and has thus nothing to do with the alcohol being iodinated in the first place.

[BOS]

Holy Shit!!!Comfirmation of suspicions by scienticians.

Someone finaly putting it in a scientific type voice.
I like it..

Halogenate the ephedrine then hydrogenate it.I get it.Sounds like hydrogenation `sept replacing ya precious metals with a halogen catalyst.(I know,Iknow it aint the same but...)

Anhydrous? I believe this has been spoken of.
Yet No-one tends to listen when it aint written all nice-like.

Orgy,Great to have you around.Now I would like some clarification on the HI concentration to byproduct/racmerization issue I was once told,as you have just replaced it with a more plausible(in my head anyway)explination pointing to free I2.Please?This is very interesting("is this the right thread?"he thinks to himself).

Make the HI first.Why?-because you can.Why not?
At the very least you could use visual indication to realise you have made at least a decent% of HI containing sollution(like or unlike that red shit Argox made up).

Cook on low heat.Why?-Because that is how the scientists do it.If Warlock can do it with sunlight so can you.What else do you have to do?
I see no reason why you cant cook it hot as fuck to produce some HIacid fast, and then let it cool conciderably before the addition of your ephedrine,and proceeding from there at an almost ambiant temp(well not quite-but still nowhere near 100c.)Why should the rate of reduction/halogenation have to compete with the decomposition rate of aqueous HI anyway?Like snatch and grab.
Are there not alternative methods of iodinating without the need for either HI or RP/PI3?Certain IODIDes perhaps?
Which points me to the HCl/H3PO4-KI/NaI system of producing something Hydriodic related.

Org,when you speak of dehydrating your HIacid, I assume you are theoretically producing HIgas and some muriatic.orrect?
Why didnt I think of that   .
Oh No,I have those crazy thoughts again.

As you may or may not be able to tell,Ive been into the cabinet again.Forgive me Im new.



Of interest to anyone who likes to fuck with electricity
and believes that Iodine and Ephedrine can not be reduced in one pot.Again,carbon is the choice.More info available if desired.
The modern electro?

Patent US4702804

[jackhole]

Make the HI first.Why?-because you can.Why not?

Because it is easier for me not to.  It saves me time and I get a great product at a very respectable yield.

I see no reason why you cant cook it hot as fuck to produce some HIacid fast, and then let it cool conciderably before the addition of your ephedrine,and proceeding from there at an almost ambiant temp(well not quite-but still nowhere near 100c.)

What is so inconvenient of heating the contents of the flask to a relatively low 100 C and allowing it to reduce?  You don't even have to monitor its progression.

Org,when you speak of dehydrating your HIacid, I assume you are theoretically producing HIgas and some muriatic.orrect?

I was not aware that one could produce MURIATIC acid!    28 degrees Baume, is it?

[BOS]

Hi jackhole,

Congrats on your large rxn.

I wonder at your need to respond to my jive???
Please do not feel that I was knocking,nor was I advising.
Simply commenting for the sake of it.

What harm is there in dropping your temp a notch, in the name of purity?I am sure your product realy kicks some ass
as Im sure many a bee`s does likewise,but why try to be scientific in writeup,yet leave it at that?Again my comment was not directed at you,as you already seem to have your shit together nicely.
 

JH-Because it is easier for me not to.  It saves me time and I get a great product at a very respectable yield.
-What is so inconvenient of heating the contents of the flask to a relatively low 100 C and allowing it to reduce?  You don't even have to monitor its progression.

Come now...You have time to reflux for 40hrs and perform a semi-thorough work-up,yet you cant spare an hour or two and
change the order in which you introduce reactants to a flask? What harm is there in giving it a go?
Or shall I just crown you as meth-god now,seeing as your system is so simple,flawless,and high-yielding?

-I was not aware that one could produce MURIATIC acid!  28 degrees Baume, is it?

How is it I seem to miss all the funny parts?
What are you telling me here?
Seriously,I am no chemist,so please tell me what happens when you take the water from HIacid and react it with dry HCl gas?I know it sounds stupid but I kinda had the idea that those hydroniums might be more comfortable around chlorid rather than iodide ions.
Have I totally misunderstood the definition of de-hydration?
Tell me,tell me I want to know how this works.

No offence meant,nor taken.

Peace.
B.O.S.

[jackhole]

Seriously,I am no chemist,so please tell me what happens when you take the water from HIacid and react it with dry HCl gas?

Why, if you took water and were to "react" (I prefer to use the term "introduce") it with HCl gas, you would create anywhere from a dilute HCl solution in water up to a concentrated 37%, I believe.

[SHORTY]

I have always thought that what you described is muratic acid or hydrochloric acid or HCl.  Aren't they all the same thing?

[jackhole]

Muriatic is a trade name, that's all.  I was being sarcastic more than anything.

[ragnaroekk]

If you vent HCl gas into HI in H2O a partial dehydration of the HI takes place - say the HCl and the HI compete for the water. So HI is freed from the hydrate and can iodinate the ephedrine more easily acting as "fuming HI" would. Lower temperature - less byproduct.

Rhodium to say the reduction step is the problematic one is plain wrong.
Read Gattermann Wieland on halogenations for this for example and realize the consequences from the fact, that NEVER iodoephedrine is found as a byproduct. Damn! Thats obvious!

[Urban_XTC]

[BullwinkleMoose]

Iodoephedrine is not a byproduct !

Iodoephedrine is 'Iodine Holgenated Ephedrine '
Is an intermediate that gets reduced to meth

[Urban_XTC]

[psilly1]

If the rxn is R-OH+H-X=R-X+H2O, R-H+ I2, Iknow I skipped the phos, but my point is, if I2 is a catalyst in the reaction to meth, why the hell does it matter if R-X is being produced, since it is goig to anyway.Does it not have to lose the damn OH group, replaced with I- then reduced to the goods. Why so much controversy about not forming Iodonated ephedrine.

[Jacked]

Why did you stop basifying at 12.8? That kind of yield whit that low of a base pH is strange to say the least.. Did you use a meter to check it?
Also that high of a yield with an interface problem is a strange thing thing as well..
muratic means marine acid, it is not a trade name

[Jacked]

Just for the record there is no such thing as a dry reaction. H2O is always introduced to the reaction. A 700 gram reaction would start with 200ml H20 in a PUSH PULL and would generate more as the reaction took place.. Again for the record , Jacked recommends a LWR over a push pull any time. The yields are to close between both reactions to give that as a reason but there is a considerable quality difference and after recrystallizing a couple times there is no difference in that area of discussion..
 As far as the birch goes compared there is a difference between product and Swim knows the difference is in the people doing it.. People subject to getting there shit from a source using RP/I2 and change to a source supplying the birch method notice a big difference and complain about it... What is actually going on is the people have gotten use to a certain impurity in there shit and when it is omitted (like from the birch compared) it is not only noticed but missed...

Jackhole, If your going to do a write up on your rxn then do it in detail, You should be wanting people to be able to follow your work them selfs with the same results. This is what a write up is for.. Not just to be bragging about the size cooks you preform.. Also you need to answer Rhodium's inquires of 95% returns on the RP.. That size reaction would have consumed 50 maybe 60 grams of RP easy.

[chronic_cook]

That post was very basic which I guess isnt a bad thing! But straight 2 E? with a plethera of mixed pills seems nuts! Especially with 250G LG RP & 840 G LG I2, What the hell, am I the only one who had problems with that teqnique? Not to mention OG 2 out the ass on my post work-up! But anyways Rhodium is right those iodoephedrines pull right through an AB and they will fuck your world up bigtime. But a complete wet rxn should clear those up, not the only problem is restraining from comsuming the waste left over from a recrystallization when you run out! But I would also like to hear more details about that omega rxn. with the amount of water you used is like a 1:1e ratio why so much?? damn, you'd think that would just take longer to get a complete rxn. Also, why didnt you just gass with HCL..that shit always worked for me...alot easier then what you did, are there any benefits in that method or did it just sound good on the forum?

[Jacked]

BullwinkleMoose, what you say about Iodoephedrine not being a byproduct makes sense but after the reaction when everything should have been converted to meth then would'nt it be considered a byproduct or maybe just an impurity?

[wareami]

Jacked: I'm going out on a limb here
Not speaking for the moose...or attempting to intercept his answer with my own.
But it's been my experience that iodoeph is the necessary intermediate to meth.
The literature backs that UP from what I've read!
Iodometh(if such a thing exists[crazy) is completely different I think and just describes under-reduced meth w/impurities that weren't given time to fully reduce.

but after the reaction when everything should have been converted to meth then would'nt it be considered a byproduct or maybe just an impurity?

I think the correct answer is neither in this case. Side-rxns take place with that substance that in turn create the impurities. When the reaction is stopped prematurely and worked UP, the resulting product will contain impurities. Any Iodo's will be left behind during the work-up.
Free Iodine from post-rxn solution can be oxidized & removed with sodium thiosulfate.
I would suspect Iodoeph to be result of an under-reduced rxn.
Yield reports confirm a lower yield of meth when these intermediates are present. Instead of meth xtals obtained....nothing is obtained because the Iodo's stay in the basified solution.
Heavy emulsion during work-up also substantiates this occurance.
Yes...less than clean feedstock will also create this but the longer cooks usually provide relief to a small degree.
That tells me that full reduction of dirty feedstock can only occur given the time necessary to counter the buffering effect that gaaks play in rxn.
Ibee's done rxns at all stages(Superclean feed) and stopped them purposely during the early LWR rxn experiments to record the yields and meth/pfed percentages.
Most bees at the time thought Ibee flipped his wig cause who in their right mind would create failure scenarios in order to achieve meth???
Well the cats outta the bag on that note and Ibee will never stop that line of investigation in order to reveal what works best under any condition.
The strength mystery sparked these early experiments.
When Iodo's are present they account for expected meth weight and yields can be used to back this up.
This is part of what compelled Ibeeware to push the time/temp & hydration envelope to absurd extremes to unheard of levels.
To this day it's difficult to expect bees to adopt that tradeoff when they can have product in a fraction of the time it takes for a full reduction.
I think you'll agree that impurities are created by side- rxns in the less controlled faster cooks.
The old journals contain references and instruction that pointed to lengthier, milder rxns producing higher yields and in higher purity.
I guess the arguement will always exist between that which can be done in half the time, producing some of what bees are after in a potent enough form to pass for the real thing.
But evidence and experimentation leads me to believe that less impurity exists in a fully reduced product because the time was taken for the rxn to proceed to completion, cooking off or fully converting those intermediates instead of stopping the rxn before that takes place.
The ancient alchemist deluxe undoubtably has been performing this rxn for longer than most and has incorporated steps and procedures that minimize the iodo's presense in the end-result.
But for anyone that performs a curbshot or a superassman style rxn....those impurities run rampant.
I guess the answer is this....
What most think is fully reduced at the first sign of meth, does not exclude that product from higher levels of impurities that when ingested/consumed have similar stimulating effects on the CNS!

Allowing the rxn to proceed past those suggested cook times has always produced a superior product with less health related cramping and impurity associated jawclenching hellrides!
Again....not answering for the moose...these are just my observations based on Ibee's personal experimentation!

[java]

One thing I learned early in the hobby was TLC. With TLC  the reaction has always been able to be followed by simply spotting the starting material and the intermediate and finish product as reference. Case in point doing meth via chloro-ephedrine (a necessary intermediate ) by monitering the choorination one would know when all the starting material was chlorinated. Followed in this case by hydrogenation which also was monitored until the TLC showed no intermediate product. So with the reference one could spot the finish product and by the rf spots one could tell if the finish product had starting material or the intermediate , also some unknowns have been known to show up, present.

By monitering the steps there is no carry over of unreacted material (minimal), and the final product is almost 100% finished priduct.

I do agree that the iodoephedrine is an intermediate product and if it shows at the end , it only says that the reaction was not 100% complete.

TLC=thin layer chromatography

[jackhole]

Iodoephedrine = Iodomethamphetamine - they're one in the same, people just choose the way in which they refer to the molecule. It's the same molecule though.