Author Topic: Super High Potentcy Push/Pull dope  (Read 38849 times)

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Worlock

  • Guest
Rhodium
« Reply #160 on: February 03, 2003, 04:14:00 AM »
First I would like to congradulate you and the Geez' on the sucessfull methamphetamine synthesis using HI without Red Phos.

Secondly - Try it, mix RP with I2, it just sits there.
The I2 slowly melts and dissipates in moist air like always, but there is no active reaction. Mix in some dry ephedrine and it might do something, but only because it can remove a proton from the hydroxode  group, still no major amount of activity will begin
 
     P4
I2  --->  I2  

             P4
I2 + 2H+   ----> 2HI

                  P4
I2 +  ROH  ----> RI + HI + 1/2(O2)- this does not go very far

Without water it is a dead reaction. you could substitute other things to provide the proton .

SwiW at one time would mix RP, I2, and E together. The reaction was started by injecting  drops of  water  into the hose that drained into the reaction flask.
This was good because it can be mixed  well before iniiating the reaction.
The other advantage was it prevented SwiW from addibg too much water, drowning the reaction, stopping it from completing in an hour.

The fast reaction was probably better on smaller amounts under 14 grams, simply because it was over sooner, and the small violemt thing was controlable,
I woud not want to see a pound of E fire off in a fast reaction, too intense, too exothermic, too much pressure and the vacuum portion would be worse than the expansile,
SwiW haa seen large fast reactions get violent appear to slow down , then come back even stronger . expand and contract several times within 5-10 seconds

There was a story, whether true or not,  about a couple who would put it in a rock tumbler to mix it super well before reacting the mixture


Worlock

  • Guest
There was a bee "fj" who at one time
« Reply #161 on: February 03, 2003, 05:09:00 AM »
There was a bee "fj" who at one time worked for an ephedrine distributer
The distributer is usually also the manufacturer.
"fj" a friend of Dwarfer said, the ephedrine came in from China, they would boil it in HCl for 24 hours. This would racimise it( convert it to the different isomers) . He also added that the ratio of ephedrine and pseudo ephedrine was 60/40 but he did not know which was the 60 and which was the 40.

L-ephedrine makes D-methamphetamine this is not configuration but optical activity. The only change is the removal of oxygen , no rearrangement occurs to change the L to D/

L methamphetamine is present in vicks inhailers, it is called desoxy-ephedrine but probablt should be named either L-desoxy-ephedrine or desoxy pseuso ephedrine . These would all be incorrectly names also.
there is
L-ephed  and D-ephed or  ((-)ephed  and (+)ephed) respectively
L-pseudo and D pseudo or ((-)pseudo and (+)pseudo)respectively

[1R,2S] or (-) or (L) ephedrine are the same
[1S,2R] or (+) or (R) ephedrine are the same
[1S,2S] or (+) or (D) pseudo are the same
[1R,2R] or (-) or (L) pseudo are the same





zibarium

  • Guest
much thanks; great illustration
« Reply #162 on: February 03, 2003, 05:57:00 AM »
without water; no rxn

what substitutes might bee worth consideration, for proton providers?

any attempts with inert mediums to provide better fluid dynamics in water substitutes?

isn't the proton doner doing double duty, in a sense, in providing the viscosity that is needed?
in rp/i, swiz felt an urge to have it sloppy 'wet' without much water, and wondered how to try.

seems detrimental, by way of possible overheating, to have a slurry so thick as to get hung up on the sides of a flask.

peace, bees

Worlock

  • Guest
I have dragged around the stick figures.
« Reply #163 on: February 03, 2003, 06:21:00 AM »



Here you have all the interesting molecules, a thick bond means the bond is pointing towards us, a dashed that it is pointing away. You can rotate the molecules individually by holding down the left mousebutton on a molecule and drag it around. Right-click and choose ball-and-stick models, animate it and whatever you want. This must make the stereochemistry clear to most.




First -L-ephedrine and D-pseudoephedrine do not have identical configurations

Second - I have dragged around the stick figures. And come ip with a very different conclusion  this picture is too simplistic,  as long as we continue using terminolgy  (D,L) (+,-)that relates to optical activity and not configuration, we will be stuck.
I have said this 2  over two years ago, repeated it many times since then, sooner or later enough bees  will get past the inital shock of seeing 4 enantomers and the discussions will quit referring to useless optical terminology. Then there will be some understanding that these enantomers have a wide range of physical properties.

It is not any fun to try and deal with stereochemistry, when the topic begins with D and L because at that point, What can be said ?
only this  D and L do not accurately describe configuration they refer to optical activity

The distributer ruins the E for our purpose when they racimize it.

There are 2 chiral or assymetrical carbons in ephedrine
22=4 isomers (enanmtomers)

and since the amide N is also assymetrical( by some authors) there can be even more 23= 16

This is not my opinion this is the present way of defining configuration

Look it up 
relative diastereo isomers (diasteners)
enantomers
Chirality




Rhodium

  • Guest
Clarification/Correction
« Reply #164 on: February 03, 2003, 10:40:00 AM »
See

Post 401416

(Rhodium: "Hermann Emde's Ephedrine Chemistry Treatise", Stimulants)
for a more in-depth discussion of ephedrine/pseudoephedrine racemization.

First -L-ephedrine and D-pseudoephedrine do not have identical configurations

l-ephedrine, d-pseudoephedrine and d-methamphetamine all have the (S)-stereoconfiguration at the amine-bearing carbon, and that's all that counts.

The distributer ruins the E for our purpose when they racimize it.

Why would they? And by what process would they racemize which stereocenter?

There are 2 chiral or assymetrical carbons in ephedrine 22=4 isomers (enanmtomers)

Yes, see below for a listing. Technically, the four are stereoisomers, not enantiomers (enantiomers are a molecule pair  differing by only one stereocenter, and diastereomers differ by two stereocenters - stereoisomers can differ by any number).

and since the amide N is also assymetrical (by some authors) there can be even more 23=16

No, that's completely incorrect. First out, there is no amide nitrogen present, only a secondary amine (but that was perhaps a typo?).

The four isomers are as follows:

(1R,2S)-1-phenyl-1-hydroxy-2-(methylamino)-propane (l-ephedrine)*
(1S,2R)-1-phenyl-1-hydroxy-2-(methylamino)-propane (d-ephedrine)
(1S,2S)-1-phenyl-1-hydroxy-2-(methylamino)-propane (d-pseudoephedrine)*
(1R,2R)-1-phenyl-1-hydroxy-2-(methylamino)-propane (l-pseudoephedrine)

*) These isomers both reduces to (S)-1-phenyl-2-(methylamino)-propane (d-methamphetamine)



I have no idea how you meant that the above molecule could have 16 stereoisomers, that is just impossible. Nitrogens are never chiral in freely rotating molecules.

Osmium

  • Guest
Rhodium, you should add hydrogens in your...
« Reply #165 on: February 03, 2003, 05:23:00 PM »
Rhodium, you should add hydrogens in your little rotating pictures, at least those attached to the chiral C atoms to make it more clear. The way it is now it seems like the angle between the bonds is 120° and the atoms directly involved in chirality would be in the same plane. Of course these carbons are tetrahedral and the angles are more like the usual 100° or so.


Rhodium

  • Guest
Perhaps I should raytrace the molecules instead?
« Reply #166 on: February 03, 2003, 09:28:00 PM »
Os: Our little molecule applet is not good enough for that, if I do what you tell me we end up with a visual like the ones below, and that's not pretty:













Molecule:

l-Ephedrine ("C[C@](NC)([H])[C@](O)([H])C1=CC=CC=C1")


l-Ephedrine

Snapdragon

  • Guest
Please pardon what may be a stupid question,...
« Reply #167 on: February 03, 2003, 09:30:00 PM »
Please pardon what may be a stupid question,
When I looked up this reference,
See Rhodium: "Hermann Emde's Ephedrine Chemistry Treatise"

was sent a djvu file,
How to open a (*.DJVU) file?
Looked on Rhodium's web-site.
Is there something that must be downloaded?

It is important to me.
Tanks lots
SD :-[  :-[

Organikum

  • Guest
the distributor racemisation story
« Reply #168 on: February 03, 2003, 10:08:00 PM »
got somehow confused by the bee telling it, Worlock.
Probably this way: The distributor cooks the ephedrine he gets from china and as a cheapass he buys it bulk, with a strong mineral acid and some nickel or zinkchloride to gain a mixture of d-pseudoephedrine and l-ephedrine.(here named in the old way for more confusion  :) ).
The ephedrine goes to canada to be sold in the US and the pseudo is directly marketed in the US.
This is technical and economical ok.
d-ephedrine is only needed in separating chiral compounds in chemistry. I know of no other use of it.

for the interested some racemisation and separation patents:

Patent US2608583

amphetamines

Patent US3970700


Patent US2797243


Patent DE2903589

separation

Patent GB804788


Patent GB297385




ORG


Worlock

  • Guest
Stereochemistry ephedrine - Elder bee philosophy
« Reply #169 on: February 04, 2003, 06:21:00 PM »
Rhodium,
Excellent, you have a quick mind. Never again will the hive be plagued with D and L
we can finally use -Methamphetamine. The chief of bees sets the standard and many rally around. The internet is a role playing situation. A chief of bees can be an evil tyrant, who hordes the glory for himself, torturing the not so adept.
 However ,
the chief bee could also assume the role of a benevolent father, who nurtures the hive and gently brings others to full potential. Willing to share the limelight and good fortune because he  has more than enough. Who needs not jealously protect his position because being confident and sure. Has no problem with stepping aside now and then to let others also have their moment of glory. Being a father who is kind and considerate to his children.  He would be the most revered of all bees , The tyrant would be tolerated, smiled at publicly, but loathed in private.

Point #2
It is often the greenest New bee that is not tainted with shards of misinformation and old baggage of past drug lore. These New bees when asking  the seemingly dumbest of questions are actually peering through a veil we put over our minds  that is full of myth and misinformation. The new bee wonders at inconsistency, whereas the elder bee has accepted it, accepted an error in perception because he is standing on the shoulders of those before. It is vital to take each bee seriously as they often will pose the question that leads to the unraveling of another mystery.


Point #3
Time to get down to Stereochemistry
Let me remark on an inconsistency I have spotted, I could quote the source , but the gist of it is:

"[R,S] ephedrine and [S,S] pseudoephedrine are the precursors of methamphetamine, and it is the position that counts."

This is only  partially correct, Alpacenturi was just about to expound up the stereochemistry of the different types of reaction mechanism , when he was interrupted.
The availability of the reaction site, the crowding by various side groups, is of vital importance to the ways with which the different types of reactions can effect the outcome of the molecule. . Simply because the rule is that secondary alcohols behave in this or that manner , assumes that other factors are insignificant like charge on nearby atom

Even though the beta carbon is vital. The groups on the rest of the molecule determine the direction  of approach, ability to attack the main chain, or a side group. This will have a tremendous effect the configuration of the final product,. In some situations, as you well know, the tendency for rearrangement is more important than initial configuration. It is possible to start with [S,R] ephedrine , under the right conditions force the molecules to undergo a mechanism that results in reconfiguration of the molecule to {S] methamphetamine.  It is a crime to mislead others away from this potential rich area of experimentation.


Point #4
You are quite correct about the amide , and the nitrogen not being chiral,. It was not a  typo, nor was it a mistake.  I used the wrong terms purposely. You gotta chum if you want to catch fish. Trolling  ls a popular term.
I want to point out that , carbon is not the only  atom that can be considered chiral. In certain oxidation states, some bonds become locked, in other they oxidation states they are transient.

I hope Alphacenturi still has the desire to continue his discussion of Stereochemistry without feeling that he is treading in areas, that are forbidden, because after all we are not here to learn  only one point of view , but to absorb the collective knowledge of the hive.

It is said, I am a rabble rouser. The truth is I refuse to be lead into narrow minded ways of thinking. I accept everything, including my self as a source of potential missinformation.
Most of all, I scoff at attempts to socially stratify the hive into cliques. Is that rabble rousing, or not? It depending on where you stand.

  


zibarium

  • Guest
we are fortunate
« Reply #170 on: February 04, 2003, 06:48:00 PM »
to have such dialog. many thanks to you all.

;)

Rhodium

  • Guest
Better pictures
« Reply #171 on: February 04, 2003, 10:59:00 PM »
Yes, you need a plugin from

http://www.lizardtech.com/download/

to be able to read *.djvu documents.

And for the isomers, perhaps this will make it even more clear to you:



It is possible to start with [S,R] ephedrine , under the right conditions force the molecules to undergo a mechanism that results in reconfiguration of the molecule to methamphetamine.

Technically - yes, practically - no. Also, you will not find (1S,2R)-ephedrine (aka d-ephedrine) anywhere but at fine chemical suppliers, and that at grossly inflated prices, as it is the unnatural form of ephedrine, and as it is not found in nature it has to be made by expensive stereoselective syntheses.

As it is very hard to convert natural (1R,2S)-ephedrine into (1S,2R)-ephedrine, you won't run into that isomer by mistake, and  thus it can be exempted from our discussions here.

You are quite correct about the amide, and the nitrogen not being chiral,. It was not a  typo, nor was it a mistake.  I used the wrong terms purposely. You gotta chum if you want to catch fish. Trolling  ls a popular term. I want to point out that, carbon is not the only  atom that can be considered chiral. In certain oxidation states, some bonds become locked, in other they oxidation states they are transient.

Yes, in rare cases, other atoms than carbon can be chiral, but as that is no issue with the stimulants we discuss here, there is no reason to confuse others by discussing that fact here and now. There are even chiral molecules containing no chiral atoms, but that is off topic. Trolling is not appreciated here, nor is posting misinformation - we even have a notice on the front door saying that such behavior is grounds for banning. If you want me to explain or clarify something to you, then please ask me to do so instead of posting errorneous things on purpose.

You are right when saying that the chirality of neighboring atoms can affect the reactions of another atom, this for example explains the difference in reactivity between ephedrine and pseudoephedrine (as you can see above, pseudoephedrine is more sterically hindered towards SN2 reactions than ephedrine as it has its methyl group sticking out on the back side. None of these things will ever change the chirality of the amine-bearing carbon though.

raffike

  • Guest
Still little confused.When l-ephedrine's OH...
« Reply #172 on: June 12, 2003, 03:59:00 PM »
Still little confused.When l-ephedrine's OH group suddenly starts looking other way ie is S chiral,the name changes to d-pseudoephedrine,why not l-pseudoephedrine,raf thought that pseudo in front of name ephedrine means OH group position difference,why l in the name changes to d.Like why l-ephedrine is right form for bees but not l-pseudoephedrine?Raf thouht that these l's and d's mean chirality of amine bearing carbon and should always be l when dealing with (pseudo)ephderine that changes to d-methamphetamine.Raf has never read anything about isomeria,could anyone suggest some document or web page something where raf could learn about that a little?


Rhodium

  • Guest
Pseudo(ephedrine) Optical Isomers
« Reply #173 on: July 04, 2003, 04:33:00 AM »
To understand, you need to discard the obsolete 19th century d/l-nomenclature of the compounds, as they do not logically correlate to any actual arrangement of the atoms in space, but rather if a solution of the substance rotate plane-polarized light to the right (d, dextro) or the left (l, levo).

Instead, we need to use the modern chemical nomenclature, developed by Prelog-Ingold-Kahn, which designates different isomers as either R or S. Here you see the tabulated names of all four isomers:

(1R,2S)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (l-Ephedrine) *
(1S,2R)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (d-Ephedrine)
(1S,2S)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (d-Pseudoephedrine) *
(1R,2R)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (l-Pseudoephedrine)

* These isomers are the naturally occurring ones, and they will both reduce to the most wanted Methamphetamine isomer as the chemical name for it is (2S)-1-Phenyl-2-(methylamino)-propane - as they all three have the "2S" thing in their name - meaning that in all compounds the 2-carbon (the amine carbon) is in the S configuration, the shape which fits best into your brain's receptors.

raffike

  • Guest
aight,thanks chief.
« Reply #174 on: July 04, 2003, 01:38:00 PM »
aight,thanks chief.


Jacked

  • Guest
Novel idea with poor results
« Reply #175 on: August 11, 2003, 02:40:00 PM »
Worlock, Nice try. You defiantly stirred up some posting. After all is said and done this procedure is misinforming if outcomes are projected as wished. This was a good shot at stimulating a group effort, I will give you that. Some good information on isomers as well came out but with no references.. To any newbees or even old bees that are thinking about giving this idea a try I recommend not wasting time and money. Time would be better spent watching a reflux condenser circulating water instead of the trunk of an old junk car..

Sorry, But Jacked rates this post as a dud.


Buckshot

  • Guest
10 grams cold for 2 weeks
« Reply #176 on: July 13, 2004, 11:42:00 PM »
Ok I have had a 10 gram batch of clean ephedrine reacting in a flask with rp and I2 and a little water for almost 2 weeks. The reaction flask has had no light exposure or heat applied.
I've been excited to even smell the contents.....(I haven't opened it yet.) Until I read Jacked's post at the end of this thread.Jacked says the reaction won't work without heat. I'd like to know why? Im asking because Jacked seems like a respectable bee who kows his/her stuff. But the post has nothing to it. Nothing to back up why it wont work. Could someone explain the bad news to me, or was Jacked incorrect?
I was sure I'd have meth with the least side reaction impuraties ever.


aia2

  • Guest
Definitely
« Reply #177 on: July 14, 2004, 02:02:00 AM »
Yes, Jacked's post comes after a stimulating discussion of stereoisomers of ephedrine, and unexpectedly calls Worlock's procedure into question.  Zibarium's posts earlier in the thread also looked skeptical, if only because no scientific analysis was done on final products.

During the discussion of the HI reduction, alphacentauri put forth a convincing theory for the apparent correlation between long, cold reactions and pure product:

Post 403630

(alphacentauri: "I think this, Worlock.", Stimulants)


So in the past 18 months have any bees tried it?  Real experimental results would be very convincing.  Worlock seems to have disappeared in the middle of this thread! (last post 2/04/03)

Buckshot: how does the visible evidence stack up against Worlock's posts?  What color do you see?  Soup or syrupy?  Are there any crystals on the flask walls?

Whether you find success or failure, details about your experiment would be great!


Buckshot

  • Guest
results will be posted
« Reply #178 on: July 14, 2004, 07:30:00 AM »
I haven't had a chance to look at the reaction flask.The flask is sitting in a dark place at a friends cottage. I'll be going there in the next couple weekends for sure, so I can give us an update. I would never leave a reacting flask un-attened under normal reaction circumstances, but that is one of the main benefits of the cold rxn. You dont need to baby sit.

I can say that the experiment was 10 grams of very clean E, 12 grams of lab grade iodine cyrstals, with 7 grams of very clean match book red phosphorus. (I get my mbrp as clean aas it gets.) I added a touch less water then I'd use in a long wet reflux. I know thats a vague description for my dH2O amount. Its been at outside temps but its been rather hot this time of year.

No light exposure, and I've read threads with hints that suggest sunlight may stimulate the reaction. I agree that ultraviolet light would help the reaction along, but my experiment is to get the cleanest dope ever using an extremely slow "cold" reaction approach. My thinking being anything to speed the reacion along including light or external heat would cause side reactions and unwanted side products. I did NOT however pre-chill any ingredients in the freezer.

The flask isn't hooked up to a push/pull system, I used a bike tire innertube cut and tied off at one end, as a reflux, to replace those balloons. A balloon works (sometimes) for short reactions, but the acids will eat through it in a day or two (sometimes in minutes), this reflux membrane has to hold up for a couple weeks. My slight concern is that my knots on the innertube will have a slow leak....I doub it will leak. I'm hoping the sides of the flask are not red color or orange but a nice golden yellow.

I've done a variation of this before, but it was because I didn't have time to do the whole LWR at once so I heated the flask for an hour then let it sit without heat for about 3 days. During this 3 days the ballons kept breaking/leaking which probably released precious gas. After those 3 days I removed the balloon and just let it "breath" at normal atmosphere for another 3 days. That batch was 5 grams of E going in and I got about 3 grams of meth back and it ws the very best meth I ever made.

Another question is what is a good method to seal off the end of the inner-tube? I just tied a bunch of vey tight knots on the end.

I should be able to tell by the smell as usual I think. Has anyone ever had that sweet smell from a flask and not had decent end product? I never have seen poor product after smelling that "complete sweet meth" smell.

Im excited about this, I will post results for sure. Cold reacted meth.....If it works I'd like to try cooling the entire rxn. Even keeping it in an ice bath during the initial exthermic reaction phase to keep it cool as possible, then  keeping it in the fridge for 6 weeks or something.


wareami

  • Guest
Not likely....
« Reply #179 on: July 17, 2004, 05:23:00 PM »
Heat is a necessary component of the rxn during the critical reduction stage.
Yes, The rxn itself will start out exothermic, but loses energy and cools off by itself.
To expect a conversion to take place under cold conditions is like wishing the sun were blue because it looks prettier than the red one.
You could leave the precursors sitting in rxn for a year and they won't fully convert without some external heat.
Some bees have reported success over time just using lightbulb heat but Ibee would bet that the reduction percentage to meth was under 70%. Just enough to feel it.
Don't get your hopes UP!
If you don't want to waste all that time and chems....apply some heat for 12hrs before work-up