Author Topic: Super High Potentcy Push/Pull dope  (Read 77644 times)

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BenWiFFen

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Sublime what?
« Reply #40 on: January 19, 2003, 10:49:00 AM »
The reason for placing your flask in the freezer and then a ice bath. Mix your dryer I2 with your P/fed chill for 5 min only. Add your r/p slowly and mix. You will have plenty of time before any white smoke never purple.


AbSoLuTe

  • Guest
Melting Point/range
« Reply #41 on: January 19, 2003, 12:27:00 PM »
Hey again Worlock, could you give us the Melting point of product and colour pre acetone/ethanol wash. Am interested as the proof isn't in the pudding, it's in the M.P
Yeah BenWiffen Worlock voice does sound different not like the old Worlock @ all. Maybe he has grown a bit, Dunno


SPISSHAK

  • Guest
I have tried this too
« Reply #42 on: January 19, 2003, 12:35:00 PM »
It does work and yeilds are good but you need a lot of time and the acid has to be super concentrated for this to work, and the red P has to be grind fine to give more surface area.
I'm too impatient for this.

cthulhujr

  • Guest
Re: The fast reaction blasted the ephedrine...
« Reply #43 on: January 19, 2003, 03:06:00 PM »

The fast reaction blasted the ephedrine into D and L meth..We have been blasting the ephedrine to both d and l meth m with a harsh and fast reaction
.




Swim is not trying to be a pest, but how does that work?
Swim thought this was a strictly stereospecific reduction.  

Illustration of the commonality of these syntheses is seen in the following
facts. Stereochemistry implicit in the first route I also applies with
hydriodic acid/red phosphorus reduction. That is, only (-)ephedrine and
(+)pseudoephedrine yield (+)methamphetamine.


this is from the 'meth impurities' document




SPISSHAK

  • Guest
This is how
« Reply #44 on: January 19, 2003, 04:19:00 PM »
Your not a pest, the reaction produces methylaziridine, this is in the cis-trans form that's where the epimerization occurs, the aziridine then gets reduced as confirmed by NMR the ratio of isomers is 25% trans and 75% cis so 25% D, 75% L isomers is a typical result.

alphacentauri

  • Guest
Hypo concentration, reply to Worlock
« Reply #45 on: January 19, 2003, 10:48:00 PM »
The hypophosphorous acid concentration I'm referring to is 50%, density (as stated on the label): 1,206. This makes the solution slightly less than 1M (one mole hypo per liter solution), or 10-3 moles per ml.
I read that water is a reaction killer, but, for Christ sake, a bit of water to bring the hypo, pfed and iodine together in touch.....or we want to react dry reagents!?!?!? :o

Worlock

  • Guest
cthulhujr
« Reply #46 on: January 20, 2003, 12:22:00 AM »


The fast reaction blasted the ephedrine into D and L meth..We have been blasting the ephedrine to both d and l meth m with a harsh and fast reaction




Swim is not trying to be a pest, but how does that work?
Swim thought this was a strictly stereospecific reduction.  

Illustration of the commonality of these syntheses is seen in the following
facts. Stereochemistry implicit in the first route I also applies with
hydriodic acid/red phosphorus reduction. That is, only (-)ephedrine and
(+)pseudoephedrine yield (+)methamphetamine.


this is from the 'meth impurities' document





Life seemed much simpler back then, too, but it created confusion and we need to be more accurate in describing configuration.
There are two chiral centers in ephedrine and psuedo
The (+) pseudo and (-)ephedrine have a similar configuration at the chiral carbon not attached to the oxygen

Ephedrine is a relative diastereo isomer (diastemer),it can exists in four non-mirror image configurations.
L- ephedrine is imported then racemized by the distributers , the racemic mix being a better nasal decongestant.

The process of racemizing the E creates a mix of isomers
Remember Ephedrine with 2(two) chiral carbons can have 4(four) isomers.
[R,R],[S,S],[R,S], and [S,R] configuration of ephedrine.

[R,R] and [S,S] are also known as pseudoephedrine.
[R,S] and [S,R] are commonly called ephedrine.

The terminology of (D,+ and L,-) refers to optical rotation, a hold over from older literature that does not describe configuration.

So we are beginning with 4 types of ephedrine that will form the two types of meth (D+ & L-) or [R] & meth. Depending on which form the ephedrine is in, will determine what form the meth will be.
The longer timed  and colder reaction allows the E to racimize again changing form,
For some reason the preferred form of E reacts more readily than the others, this creates more of the (D+) or [R] Meth, when  under the milder conditions.
The fast reaction did not allow the E to change form it  just reduced it all retaining the fornm it was in.

To confound the issue, the reaction is a two step  SN2 reaction with the formation of an intermediate carbonium ion (Alcohol addition of a halogen)
This type of reaction is not stereo specific.
However.
It seems that the size of the iodine prevents the bonds from rotating at the moment of reduction of the ephedrine.




Worlock

  • Guest
alphacentauri
« Reply #47 on: January 20, 2003, 12:44:00 AM »
Check your Private Mail


morpheus

  • Guest
Congratulations Worlock
« Reply #48 on: January 20, 2003, 08:09:00 PM »
About 2 years ago Curbshot and Super Ass Man(where is he?) were trying to come up with a sure fire no fail synthesis
for the Newbee,that would guarantee some product.It looks like you did it,and without fire(heat).Of course they could always screw up the a/b or gassing.Oops forgot about cleaning the precursors too.Anyways the reason for asking for your old post was a friend is interested in rp/hi reduction.Swim can't begin to tell him in laymans terms
whereas you have a rare gift of communicating chemistry
so a grammar school kid can understand it.Thanks,will let
you know results of my dream.

methylaminorex

  • Guest
@WORLOCK
« Reply #49 on: January 20, 2003, 08:47:00 PM »
good work  ;)
how about if the rxn does not fire off from self?
should one use some heat to start bubbling, before setting the flask aside for 4 days?

methylaminorex

  • Guest
up :)
« Reply #50 on: January 20, 2003, 11:05:00 PM »

handsfull2

  • Guest
incubator
« Reply #51 on: January 21, 2003, 05:32:00 AM »

handsfull2

  • Guest
huh?
« Reply #52 on: January 21, 2003, 07:26:00 AM »
Ok moderator''I see your having fun with the buttons again huh.


I was merely trying to help with some sugestions on how to keep the rxn warm while waiting for the 4 day time limit that worlock suggested in this thread.

seems a egg incubator would solve the problem of maintaining a constant temp'' and the egg turner would slowly keep the rxn moving while beeing incubated""so what part dont you understand?
   :)


Worlock

  • Guest
How to screw up
« Reply #53 on: January 21, 2003, 03:04:00 PM »
The simplest and most popular way to screw up this reaction method, is  easy to do  and easy to fix. Is the addition of too much water.
I know we think of a reaction as being wet, but this reaction must be started out dry, it gsts wetter as time goes on.,

How dry is dry
When the E and I2 and RP are put together it should be so dry and thick of a mud that when you roll the flask slowly the reactants barely move at room temperature. within a minute the reactants will begin to fire off.  At this point you can roll the flask slowly and the mud begins to flow and mix together, you will feel the heat being generated through the flask. Keep rolling the flask you will notice that rollong it slows the reaction dowm.
 
If none of this has happened and the reactants are still stuck to the flask and look dry add a small amount of water, if doing under 1/2 ounce you might add four drops of water. If doing over 2 ounces  add 2 ml of water.
If the reactants flow while you roll the flask, but there is no white fog or heat or bubblingm then give it a blast of heat, until it bubbles.

Once it is mixed and the smoke is starting to escape from the flask. then put on your stopper and hose.



Cold reaction
In the cold reaction. you are done for now, just keep it warm and mic it when you get a chance over the next few days.

fast reaction
In the fast reaction, when the bubblimg dies down, add heat, until it gets all turbulent and blows gas(185 F) After the gas expands it sucks it back in violently . you are done with the reaction. let it cool.  add water bring it to a boil then fllter out the RP.

Too much water
If you added too much water, and did not see any of the reaction signs then gently heat it, without the stopper, until it boils. Maintain the boil with out the stopper for 1 to 4 hours until most of the excess water is  gone. It will be a thick soup, that does not stick to the sides if the flask. When swirled it runs down the sides within a minute. At this point the reaction will be completed, add water bring to a boil and filter off the RP.  




placebo

  • Guest
I'll see you in 4 days!
« Reply #54 on: January 21, 2003, 04:07:00 PM »
I'll see you in 4 days!
One question, you spoke of quality, what's the yield like? I assume no worse then before.
Good to see you back master!


Jacked

  • Guest
Water ratio
« Reply #55 on: January 21, 2003, 09:49:00 PM »
Use 5 Ml H2O per 28g starter. add 1 ml for walls of the container holding the calculated amount of H2O sometimes 2 if it is say a 125ml beaker but the ratio is ample enough water..

During the regular P/P event one will wonder if they added too much H2O at these ratios but just don't rush it. It always reaches 2en phase. I don't see why the same ratio wouldn't work here...

Swim knows some will have a problem controlling the starting of this reaction, normally Swim doesn't mind the first phase reacting so vigorously after it has mixed and molted to chowder with no heat being applied but this time he felt it would be to hot.  A S/S bowl with crushed ice and acetone had to be used to slow down this event. The idea of adding acetone is to help the thermal transfer of temp through the glass happen at a faster rate because by time the eye sees the need for cooling it's late, cooling needs to go down quickly due to the eye lag thing. It takes a little bit for the contents to see a temp change and settle down for you..


Worlock

  • Guest
"...the result was very potent..."
« Reply #56 on: January 22, 2003, 08:26:00 AM »
Here is a Bee describing the results of cooking meth a second time.
It indicates  that there is probably unreacted E in the product.
Not only that but the E is undetectable by tasting the product,
A longer cooking time should convert more of the E to Meth.


In reply to:[Worlock}

Its interesting that you mentioned cooking a second time.  A few months ago, i was doing alot of reactions, at least 2 a day and was not getting very good results.  Then one day i ran out of pseudo and thought what the hell and just tossed all the meth which wasn't very potent in a flask and rereacted it.  The rxn didnt take long and after steam distillation and titrated which was alot easier to do compared to first cook. the result was very potent. i assumed that i had not been getting the pseudo clean enough the first time.  Never thought about it being the isomer.  anyways from then on I always keep all the not very good meth and rereact it.  So far have never been disappointed. 
Thanks again for your reply.





Worlock

  • Guest
Absolute
« Reply #57 on: January 22, 2003, 09:13:00 AM »
Sorry I don't have a melting point apparatus.
I do agree that the proof is in the M.P. and in the abi;ity too obtain a good sharp melt, Nothing is worse then 1/2 of it melting too soon and the other 1/2 melting too late.

A polarimeter would be great also, a home made version would be easy to make , except locating  small square sample containers



AbSoLuTe

  • Guest
No MP apparatus?
« Reply #58 on: January 22, 2003, 10:29:00 AM »
Do you have 'Organic chem lab survival manual' by Zubrick?
It has a very simple 'apparatus' for doing an M.P.
I suggest you buy it or go to a library or download a copy of it. You should have all the equipment and expertise, worlock.
Waiting your results.


AbSoLuTe

  • Guest
As far as half melting to soon and half ...
« Reply #59 on: January 22, 2003, 10:40:00 AM »
As far as  half melting to soon and half melting to late goes , YOU HAVE SHIT OR NO METH.If it is your product then it should melt at exactly its MP and within its range, which if I remember correctly is 172deg C(correct me if I am wrong) I have been given and bought stuff that was guaranteed to be pure, straight out of the gasser to the dryer, or stuff made with the Hypo method and uncut and it is not MethAmphetamine, It may well be something similiar to it or it might contain small trace compound of it , but it IS NOT meth.
The only (simple)true test for purity is to do a MP, unless you have access to a Analytical Lab
As they say, garbage in garbage out.