The Hive > Stimulants
"True Blue" NH3/Li reduction ie birch
ordinaryguy:
This process assumes the reader has some experience regarding a NH3/Li reduction of ephedrine hydrochloride or ephedrine freebase. The quantities of reactants listed are based on 60 grams of clean ephedrine freebase and the presence of any contaminants including waxes or fillers will change the quantity of NH3 and Li needed for the reduction to complete effectively. Please use caution when manipulating the molecular structure of a compound. They enjoy attentive handling. Please read material safety data sheets on all reagents in the processes prior to attepting the process. This basic list of instructions excludes much important data regarding the safe handling of reagents.
A good education is the best safety coordinator.
Please take time to read accordingly.
The BIBLE says in James 3:8 "But no man can tame the tongue. It is an unruly evil, full of deadly poison."
Having all that been said lets get on with it.....
1- add 500ml of NH3 to rxn vessel
2- dissolve 5.5 double a Li strips into NH3 1/4 a piece
at a time taking approximately 2 minutes per while
stirring or swirling. 15 minutes later you have a deep
indigo blue solution with the consistancy of a thin
soup. If your rxn vessel is not on a ice bath you
will loose a substantial quantity of NH3 in this
process.
Adjust accordingly at the onset of process.
3- slowly, add 250ml of NP
solvent/ephedrine freebase solution to the rxn
vessel stirring or swirling the entire time. The NH3
will displace the NP solvent allowing the Li to
manipulate the ephedrine reduction directly to
the freebase molecules. This will hold true as long as
there is adequate quantities of NH3 present to displace
the NP. The coolness generated by the NH3
stabilizes the freebase molecules during the reduction.
4- remove the rxn vessel from the ice bath
5- continue stirring or swirling every 2 minutes for a
full 15 minutes. This will assure all molecules of the
freebase have interaction with the Li which is the
reducing agent.
6- remove top of rxn vessel if fitted and allow
evaporation of ammonia to begin.
7- Add 250ml of anhydrous NP. Note: if NP is warmer than
room temperature the evaporation of ammonia will
accelerate synergistically. Some consider this
benificial as the reduction has been completed in the
first 15 minutes and the balance of the time spent
is waiting for the excess ammonia to evaporate. This
usually takes about 30-45 minutes but can be done
quicker via DH20 washing.
8- filter off the reaction fluid being careful not to
include the solids remaining in the rxn vessel.
9- add 100ml hot NP solvent to rxn vessel and agitate
for 5 minutes. This should gravitate any freebase
molecules trapped in the post reduction waste and the
NP solvent. Let settle 5 minutes then filter again.
10-with a gloved hand placed inside a pantyhose
stocking, collect the solids from the rxn vessel.
squeeze these thoroughly through the stocking, above
the filter into the collected solution until no more
liquid is released.
This may contain some freebase oil.
11-add 250ml hot DH2O to the NP/freebase solution. Shake
violently for several minutes. allow to settle for 10
minutes. remove the aqueous layer. now add 250ml cold
DH2O to the NP/freebase solution shaking violently
again for several minutes and allow to settle for 10
minutes. remove again the aqueous layer. a third DH2O
wash will get any residual water soluable contaminants
such as chlorine or NaOH out of the solution.
12-now you have two choices. either gas or titriate. then
evaporate or filter and acetone crash and recrystallize.
13-lucky thirteen! 95% pure product at a yield
of 78% the original mass in weight. 60 grams reduced to
47 when the a/b was clean and all filtering mediums were
pre-moistened. swims preferred a/b extraction begins
with a DH2O soak then taste test filtering prior to NaOH
push. the NP/freebase solution was then succesively
washed 3 times with DH2O. the NP/freebase solution was
then reduced to 25% under very guarded heat(low, low,
low). the NP/freebase solution(anhydrous) was then
slowly added to the rxn vessel during the reaction.
the one drawback is wondering how much product you have
in the NP/freebase solution.
swim feels the uncommon yields are due to the minimum
use of filtering agents and lack of handling the
crystalline product. this combined with an accurate
Ph level during the NaOH push is pobabably the
explaination.
A) the NP/freebase solution was created during a a/b
extraction of a pill solution that was filtered
prior to the NaOH push. then three successive DH20
washes were completed prior to the 25% reduction
under low heat. this made for a near crystal clear
solution of NP/freebase stock for the reduction.
B-the whole process took just under an hour. rather than
wait for the ammonia to evaporate, swim chose to do
3 successive DH2O washes to remove the ammonia, chlorine
and NaOH reminants. the Li was spent in the reduction
process while the NP was retained with the additional
amount that was added for the final titriation/gassing.
also it should be noted that the original pills had a
antihistimine listed under active ingredients. swim
believes these 2mg per pill were either diminished in the
rxn environment and released as other by-products or
account for the 5% impurity.
swim prefers gassing to retrieve HCL needle like crystals
and uses these without acetone crashing or
recrystallization. swim believes these steps to be unnecessary having little or no affect on the final product.
swim also conveyed a therory she has regarding rxn's that are interupted by the addition of DH2O. She theorizes that the DH2O/Li rxn creates an environment that propels and encourages over-reducing. She believes pockets of concentrated Li are accumulated when the DH2O/Li interact creating an environment in which the temperature exceeds a favorable level for the stable reduction of the freebase molecule. The result being small deposits of over-reduced or otherwise damaged molecules. She also stated that the only time she would consider interupting a rxn with DH2O is when there was an excess of Li known to be added to the rxn due to the lack of a scale or having previously failed to identify the required quantity for the rxn to complete. she then would add DH2O because too much Li IS known to cause over-reduction and/or molecular damage. this would result in smaller yields and a less favorable quality. she also has a theory on multi-solvent extractions, alchohol extractions and NP soaks, adding moe contaminants than they remove but we won't go there.
all I know is that swim knows her "True Blue" like a true crystal knows it's proper structure ratio!
the rest can just vaporize..............
weaz1dls:
I read through this quickly a week or so past and did not notice until this time that the diference is the addition of freebase suspended in NP. This sadly has been standard in the past. I do share your excitement and joy for nailing a smooth procedure. Due to the nature of NH3 and it's availability not many opt to Birch. SWIW believes it to be fabulous but alas lack of patients and the existance of close neighbors keeps this dream at bay. Also keep in mind that quite a few Bee's are having dificulty with pills and your joy may not be welcome company. Though this procedure may seem in your eyes to be the answer for those Bees, time will tuely be the judge of that. As most of us are sceptics and believe sucess under any reaction to have it's numbered days until the pill fuckers roll out a new beast. Again congradulations and if you have any tips for the micro bircher toss me a PM. ;)
WizardX:
The quantities of reactants listed are based on 60 grams of clean ephedrine freebase and the presence of any contaminants including waxes or fillers will change the quantity of NH3 and Li needed for the reduction to complete effectively.
--- End quote ---
The ephedrine freebase MUST BE DRIED before using in a birch reduction as ephedrine forms a hydrate (ephedrine.1/2 H2O). The water on the hydrated ephedrine will react with the Li and diminish the mole ratio of Li.
ordinaryguy:
I believe it was mentioned in the original post that the NP/ephedrine freebase solution became anhydrous while reducing the quantity of solvent over low heat. If the solution was not properly "dryed", there may be enough moisture to react in a way that was less than pleasant when it came into contact with the dissolved Li(not to mention changing the rxn ratios a tad) This moisture content is stated to change the ephedrine to a hydrate. That would lead swim to believe that it has become a new compound and that a rxn would be necessary to free the ephedrine of the H2O. I am not a chemist by any means nor is swim. Possibly the addition of a heat source above H2O's boiling point but below the NP's flash point would be in order. If not youv'e got me cuz swim continues to stand by her original post verbatim. Swim is curious as to whether or not you are suggesting that something other than heating need to occur to properly dry the E. Thanks for the response. I appreciate.
ordinaryguy:
Hey weaz
Thanks for the thata girl, guy or whatever. I can relate to fellow bee's frustration with extraction inhibitors. I am not sure if swim remebered that these bee's collect honey all over the globe. Sometimes it's easy to assume flying is as easy south of the equator as it is north. Sounds like somebod-bee should post a simple, effective pill extraction technique for the fellow swarmers. Maybe swim has a copy I could post. She is kinda scared of the internet with emails and all required. Personally I don't have anything to hide(other than my stash) I think I'll get a PM to ya sometime in the future. I watched swim perform this rxn on 60 grams in a basement one bedroom apartment without incident. Very confident she is. Not only that but with all the necessary materials needed sold OTC you may just convert with a little coersion. At any rate thanks for the post. I was sure that somebod-bee out there had used suspended freebase before, I was just suprised not to see any posts on it. After all, it does save a substantial amount of excess handling from being required. Any tips on how to create image files so I can send you some good nano pointers?
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