Birch Baby

[Jacked]

The Birch is a cool fucking reaction and is quite easy to do. Swim has 5 under his belt now and am real happy with the results from each one of them... Using a 3L Elmira flask he now adds approximately 120g's pseudo that has been alcohol extracted and cleaned with xline, Naphtha and acetone boils until liquid comes off clear, usually just under a gallon of each except acetone which takes a full gallon usually.. The pseudo is clean enough for a RP/I2 reaction so it glides through a birch.. With the Pseudo in the flask and air mask in place with good rubber gloves up to the elbows he lays the tank on its side with the opening of the valve pointing up then he opens the valve slowly with his hand cupped over the mouth of the flask with the nylon hose between his thumb and forefinger just until the initial gas is released then the liquid comes without disturbing the pseudo, He lets about 600ml collect then moves to the fume hood were a S/S bowl semi filled with ice, and acetone, sits, He places the flask in this and inserts a plastic whisk attached to a drill motor held in place with something that looks very unprofessional to say the least.. He has 44g of Na in a small S/S container covered with Naphtha sitting inside the same set up the flask is in. The metal gets cold as hell and when added over a period of only 10 min while stirring does not foam up near as bad as it does at room temp... The stirring continues and after another 10 min. the reaction turns dark blue almost black, At this point the time is started and the blue is stirred for 30 min... The reaction is quenched with small amounts of H20 squirted into the flask, It doesn't take but maybe 6 or 7 ml to make the blue go to grayish white. He is thinking about using iron fillings next time to quench with instead of H20 just in case of unreacted Na that might be lurking about...Next about 500ml of toluene is added and the bubbling is started. It takes about 4 to 5 hours for all the Nh3 to leave the flask completely. A teaspoon of Sodium hydroxide is added to see if any more bubbles are produced and is done so until no more release of bubbles are seen.. Then the mix is vacuumed filtered and separated followed with a few good H20 washes followed by titration and evaporation of approximately 100g's of clean white sparkle gear that is expected from a good reaction.. Swim is damn sure hooked now... The first time he let the smelly out of the bottle it tingled the upper arms almost a burning sensation of the upper arms that was uncovered and a then a bit penetrated the mask because of the harry face not being shaved scarring the shit out of one cave man.. That is some powerfully stuff. Once the flask is in the fume hood the mask is removed but that was only the last two times. The first couple of runs you couln't pry that fucking mask off.. What a trip... I'm fucking thrilled with this and cant wait to do another one...

[Jade]

Nice write up, Jacked.  I have a couple of questions though:

Have you ever done this with Li instead of Na? 

He is thinking about using iron fillings next time to quench with instead of H20 just in case of unreacted Na that might be lurking about...

Excuse my ignorance but what do you mean by "iron fillings"?

[mnm]

Excuse me for interjecting, but iron fileings are just small pieces of iron shavings my love.

[Jacked]

Yes a long time ago Largeman came down for a visit and we ran my first birch. We used Li because it was the thing to do I guess... Li can over reduce the pseudo and there is a great concern around how much time in the blue one should have to get a completely reduced product without over reducing it resulting in an unsavable product (so I'm led to believe) When Na is used it is said to only reduce one step (not quite sure how to say what I mean) being more forgiving to an extended reaction time. (Something in that order anyway).

Iron turnings or fillings is just that, Take an old cast iron skillet and rake a file across it collecting the shavings or drill a hole through it collecting the turnings (chips). This is said to quench a reaction just as H20 would, See, H20 and Na do not get along at all resulting in a britte red and very hot fire that is cool to see in a mud puddle but not in a flask with 400 ml or so of solvent. Not to mention the gear

[xboXer]

The way you fill that flask is damn scary! Get a nipple for the tank, stainless, some poly or nylon tube to fit. get a stopper for your flask, bore 2 holes in it. now get some flexi tube, (vinyl) cut one 5" and one 10" piece of stiff tube put both in the stopper. use the flexi (vinyl) to connect from the tank nipple to the 10" pc. use hose clamps to snug securly. Using a long length of vinyl, connect to the 5" pc and the other end shove down a drain or into the toilet, past the trap. If that isn't doable, run an exit tube TWICE the ID of the tank tube, and run it up a tree, pole etc. 20-30 ft. now the AA can flow into the flask, and the fumes are vented out of the general vicinity of the reaction. Make damn sure there are NO kinks in the lines when setting up...

[Jacked]

I have a s/s ball valve that has the Nh3 tank fitting on one end screwed into the tank, a 1/4" s/s covered nylon tube runs from the tank to the flask... "Hose in between the thumb and forefinger" should have been the clue..

[xboXer]

Thumb and forefinger reads as though you are simply holding the tube in the flask w/o a seal. The part where fumes got past the seal of the mask due to beard stubble, and the mask is removed once the flask is in the fume hood. Tingley sensations? reads as though you have an OVERabundance of fumes contaminating your space outside of the fume hood. Needlessly. AA is so water hungry it will actually RIP water molecules from any part of your body it contacts, hence the tingle. When I fill a flask you don't even know it. AA don't fuck around. Just bee careful.

[Jacked]

The Smelly quickly leaves the room and sense I have shaved underneath my chin I have had no problems, The air source is self contained. Nh3 is dangerous and sense only one gram of the gas takes up the same amount of air space as 22 2L coke bottles would, it doesn't take much to get a tingle from it. I understand the hazards involved and I thank you for your concern for my safety and anyone who might read this thread as well..
The bottle Swim has leaks from the packing when its open and the seal area is old and rust pitted so getting a good seal from the fitting that was made for this bottle is damn near imposable, The fume hood is not big enough to accommodate the bottle but the vacuum in the room itself evacuates its volume about every 45 seconds. Exhaust is the most important thing besides a good powder and co2 fire extinguisher handy. Also Swim has a 6" round x 1/2" thick rubber with a handle to place over the flask in case of a fire during quenching. That about does it for the safety gear, I should have covered this in the first post, My mistake.

[beez_neez]

The birch has become Swibn's preferred method over recent times. Quick, easy and great yeilds. Swibn mixes his annie and Na in one flask, a little annie and fb in another, then slowly adds the blue to the fb/annie flask.
Upon addition, the blue will dissapear almost instantly. But when rxn is complete, blue will hold for around 40-60 seconds. This cuts time down considerably.
Then Swibn adds NP, followed by dh20. The layers can bee seperated immediatly and the water/ammonia layer discarded. Quick wash of NP with a little more dh2o, seperate, dry NP, filter gas and PRESTO!
Swibn has his time down to just over an hour.
Give it a go-go. You will bee most impressed.
This method also reduces the chance of having any unreacted Na in ur mix.
And yes, Na is the best way to go.

[dwarfer]

if I were you instead of adding squirts of water,
I'd fling in an ice cube or two.

The monia trys to keep the water from going liquid,
but the metal wins every time, and the reaction 
ceases, white returns, and vaporation time begins.

Without trying to totally replicate what I think
Marvin  said here before, but trying to save your
 precious ass for those around you who love and
admire you yadda yadda yadda..

Use a two hole collecter like a heavy duty filter flask,
or heavy duty ehrlinmyer.  Run the smelly down to
the bottom or near it with a glass tube, and
have the "suction nipple" connected up to a tube
that is held under water, or better, a weak HCl
solution.

Now when the smelly runs in, the gas gets pushed out
 and gets absorbed by the water, making amonium chloride
if you have dilute acid, which you should save because
maybe someday you will need some.

For example, IF YOU REALLY WANT TO QUENCH THE FUCK
OUT OF THE REACTION like " NOW", FLING IN THE
AMMONIUM CHLORIDE YOU MADE LAST TIME..

but really, the ice cubes work mo' bettah.'

so ANYWAYS, now youse gotz a tub full of cold 'monia,
and NO smells, and NO burns on you punkin 'lil'hands.
VIO(fuckn)LA!

Tell you MOMMA to give you KISS fo' ME!



PS PS PS PS PS :

Now once you done RUN the monia in da JUG??
disCONNECT the blow hose what leads to unner da wa wa.

Why? After WHile, it SUCK back water as de MONIA
fumes go away an da OVER capcity section heatz back up.

now DAT sux fer SHURE!

parTICUlarly if you got dissolved METAL in da MONIA!!!

trust ME on DAT one.. 

so ANYWAYZE again, if you just DON"T think you can disconnect the hose in time..
(Like 30 seconds DUH)

put in an INTERMEDIARY sealed jug soze that a SUCK
back would land DERE instead o back in da
collection vessell.

(DISCLAIMER)  Marvin told me to put this up, and
I tried to use his disgusting brogue/dialect/
pidgen english, but I could not duplicate the spray
that he always subjects me to as he talks too loudly
 thru his two missing front teeth. Which he also holds
his cigarette with.

Anyway, it's probably all lies.

[maple_honey]

Well I'm using Li here and it seems to be fine. You only need to use about a quarter as much because of it's atomic weight and it seems to be acquired without huge hassles. I guess Na can be made from lye so it might be the best way to go if no Li is available.

I noticed that when I use too much Li, reaction has a tendency to stay black for quite some time. I've added a little more FRED to get it back to the light greenish-yellow and then ultimately to the dirty white color. Now, if one simply follows the 2:1 molar ratio to a T, then isn't the risk of overreduction zero?

I add my FRED and my AA first. Then when everythings sitting around -50C, add in my Li, put on my overhead mixer, and let it go. Is small additions of Li better? It's more of a hassle. It seems to all react OK and doesn't boil over. Usually only stays black for 5 minutes or so, turns to yellow, then to white. I let the reaction go a half hour and then let the AA evaporate under some light heating.

It seems like I need a shitload of toluene to get out all the finished product. Is camping fuel a better NP for this step? THF is more difficult to get.

Also, once I have all the freebase honey in the np, I usually put under a mixer and slowly add muriatic acid until pH is 6.5-7.0. (I could dry gas but vacuum filtering is a big hassle if I'm not keeping it a powder anyways). Then I extract the salt with water and boil down the water to a cake. Trying to convert the cake into shards but I haven't got this ICE thing down yet. Take up in denatured and acetone to try the "Dual Solvent Crystallization" but it doesn't seem to work.

QUESTION: Can I skip the water all together and use denatured alcohol and the NP with freebase together in the sep. funnel? Then add enough HCL to make my pH 6.5-7.0 to migrate the salt into the alcohol? There would only be a small amount of water in there then from the muriatic acid and I could go right to the alcohol boil down for recrystallization. (Assuming it actually works). NP and ethyl alcohol would seperate as far as I know right? Ethyl is polar I believe.

By the way, before someone does the UTFSE thing again, trust me, I have.

[Jacked]

Well now, I like the double dipper flask stopper and water bucket idea..

#1 about dissolving the Na in a separate container to me seems like the electron field is already working before it even sees anything useful to reduce. That's just my picture of whats up, I could be way off here.
#2 Swim has recently come into contact with gear made this exact way by a well known bee. The taste of unreacted ephedrine is very evident and after an exchange of happy juice this bee's eyes opened and conformation on quality was given.. I would hate to re event the wheel. It will take a bit more convincing for me to change to that method but keep in mind I am a new bee at the birch but I still got a hard head.

On the question about toluene and camping fuel.. Stick with the toluene or try xline but the Colman's is like naphtha and mite need a little warming to get the goodies to migrate, toluene is the best or next best thing in my opinion. 
As far as Na and Li, Na would be the best way because of it only being able to reduce by one instead of Li that is capable of ruining a complete batch..
Na can be had with out making it. I think I would use Li over the thought of molten lye and electrodes working up little balls of the stuff.. Li would be the way to go defiantly. Swim has ran a Li/Nh3 batch with another old time bee a while back and noted the sludge blue  substance left behind by that Rxn, using the metal there is a substance left behind but its cleaner and not slimy. And to avert any clean comments after ones Rxn, the shit left behind is H20 soluble and using this with solvent to extract the goodies would leave a clean appearing extraction wast.

By the way, the duel solvent recrystallization does work and is very simple to do, I don't know why you would be able to run a successful Rxn and not know how to precipitate a crystal.

A cake? Your not boiling this meth water to get the H2O off quickly are you? A small container maybe? A cake? The only cake type formation I can think of would be in a buckner's funnel from a final cleanup with acetone of a product that was gassed instead of titrated. That can leave a filter cake. 

And last but most important about the method of your crystal cake, You never said anything about washing the non poler before titrating. I hope this is an over site because it is a very important part of the process. It should never be left out of any description of extracting if not for your health then to save from misinterpretation by new bees.

I'm not being a smart ass I promise. after reading what I've wrote it kind of comes off with a smart-ass feel. It is not meant too. I'm Jacked and am moving so fast ahead, everyone I see appears to be moving backwards...in my head anyway..

[dwarfer]

Jacked you always sound real clear and unpretentious to me.

Li an Na both do the sme thing, as far as I can tell.

Although I agree that the metal flung into the precurser/NH3 seems to have a stronger reducing effect than
pouring in a solution of the already dissolved
electrons and ammonia, filtering out the undissolved metal,
dissolving it first makes the reaction complete really
quickly (just drip in the blue/black  fluid  while mixing, and as soon as blue remains, you be done.

Also, with lithium, it seems to me that it is fairly easy to
over-reduce with the bare metal being flang in.

BUt Marvin never noticed it with Na.

For sure the "reaction cake" without the metal is less junky, but no big deal either way.

For separation, steam is the best in my opinion:
room temperature  naphtha is second. 

Xylene is next.

Then you start basing the reaction cake with
sodium carbonate and re exract with Xylene,
and finally with NaOH.

this latter will yield mostly unreacted precursor.

=====================

You are right about washing.

Nothing should be gassed or titrated unless it is absolutely clear.

No whitness whatsoever.

Filter until it is clear.

[placebo]

Jacked, in my limited experiences with the Na Birch, I have to concur with Dwarfer 100%. Pre-dissolving the Na has the benefit of reducing possibilities of hotspots. Reducing risks of explosions. (Even when you think your careful, it's easy to fuck up with Na, I know!) The electrons aren't wasted as there is nothing for them to reduce until you add it to the mix. (Save for miniscule amounts of moisture from the air.) The whole procedure seems faster, smoother, easier to read, cleaner, safer when done this way. It also gave me higher yields.

I aint saying there is anything wrong with what your doing, just saying give it a try, you won't be dissappointed.

[fanofshulgin]

A bit late in pointing this out, but 1g of NH3 will occupy 1.3L of volume, 1 MOLE would take up the 22.4L.

[Jacked]

I wasn't sure about predissolving the metal but I will try that the very next time. It makes good sense now that I know I wouldn't be wasting energy. Dwafer didn't explain that to me, bad Dwafer.. Just kidding. I will try that out and report the results back here..

A mole does it then. I must have been misinformed or just remember it differently, I remember Mr. Cleans post that it was in just lost some details. Sounded good anyway.

[dwarfer]

They get into your supplies, and next thing?

[maple_honey]

[maple_honey]

You are actually quite correct and I feel a bit redfaced. I did neglect to water wash the NP extracted freebase and there is probably some lithium salt in my finsished product. So I freebased, extracted, and washed again, titrated, water extracted, and boiled down - and you know what - SHARDS!!! I made this mistake because I am accustomed to vacuum distillation where it wouldn't be an issue. However, it is unnecessary, it seems, with this product if it is cleaned up properly. I wonder if yields would be better or worse?

Although, the shards aren't quite as nice as my buddy's HI method but this method's ingredients are easier to get and supposedly have better yields.

Now, this is my thought on over-reduction. If you pre-dissolve the Li or Na in the ammonia first, then drip in the goods, isn't there going to be an excess ammount of dissolved Li present until ALL the suzy has been added? Wouldn't that result in overreduction because of the excess Li or does it not happen that quickly?

Now, I like the idea of pre-dissolving the Li seperately first and then slowly pouring it into the FRED freebase but the problem is the rate at which the NH3 wants to boil back into a gas. Pouring this out of the air can cause a big mess to say the least. Some type of chilled pumping mechanism may work well.

Now I hear that when this Birch is done properly that you should get close to 90% w/w of finished product back which is almost 100% molar yield. Anyone had these kind of results? Buying black market FRED is very expensive these days and to turn a proper profit an excellent yield is necessary.

[beez_neez]

you pre-dissolve your li/na, then add to your suzy flask. Swibn dissolves in ice bath, then pulls flask out of bath and slowly pours the blue into the suzy flask. upon addition, he places a gloved hand or stopper over suzy flask which is snug in  his dry ice acetone/meoh bath.