The following is a simplified street version of the Nazi synthesis. (Li~NH3)
Before we get going on the fun stuff lets talk a little about the reaction, the chemicals and there relationship to one and other.
The ammonia’s job is to melt the lithium & act as an amine , try not to be excessive with it. In the reaction below it will be in excess because of the small amount of pseudo to be reduced. The rule of thumb is 250 ml of ammonia for the first 4 lithium strips & 100 ml for every 4 strips after that. It’s possible to do with less but these aren’t reagent grade chemicals.
There must always be enough lithium present in the ammonia to reduce the pseudo.
The ratios are 1 AA battery strip for every 7 grams of Ephedrine or Pseudoephedrine as a salt.
Some say put the pseudo in fist; some say put the lithium in fist. This reaction will have the lithium in fist.
When the lithium is added to ammonia it terns blue & is smooth on stirring, When adding the pseudo if after vigorous stirring the ammonia becomes thick or the blue color fades stop adding pseudo because there is not enough lithium present to reduce any more.
This is very important when doing big reductions.
The Ephedrine or Pseudoephedrine must be dry of all moisture; this reduction is very susceptible to degradation, SO NO WATER OK!!
The lab equipment has bean chosen for ease of acquisition & reuse
Clandestine laboratories often have individuals untrained in the handling of dangerous chemicals, so be careful.
This synthesis has risk of poison gas, explosion & fire.
The handling of anhydrous ammonia is an extraordinarily dangerous activity.
The liquid is extremely cold & the vapor is highly volatile. Contact of the liquid or vapor with the skin, eyes or mucus membranes can scare for life so be careful.
The Shopping List
Chem. Gloves that go up to the elbow.
Full face respirator with relevant filters.
* Docta often uses an emergency miner’s respirator that fits in the mouth & a glass lens scuba mask like the ones on old James Bond movies.
Bucket of water as a safety wash.
Pyrex jug. 500ml (reaction vessel)
Pot from the kitchen that the Pyrex jug fits in, (acetone bath)
Separation funnel. 500ml
Oven baking tray.
Shot glasses (6)
Glass steering rod.
Glass beer or Coke bottles, (6) (just because there handy)
Plastic funnel. (Glass if possible)
Portable cooler, (to put the dry ice in)
Tools to strip batteries, (mini pliers & wire cutters)
Garden weed sprayer, (6Ltr) (HCI gas generator)
* the one with the pressure relief valve on one side a hose on the other & a hand pump on the top. Make shore the pump can be disassembled.
PVC fitting (for the gas bottle)
Clear plastic hose (1m) long about 12mm OD
Roll of paper towel.
Anhydrous ammonia, (bottle of gas)
AA Lithium Batteries. (4)
Ephedrine or Pseudoephedrine. (28g)
Dry ice, (little pellets not the bricks)
Hydrochloric acid, HCI, (strongest you can find)
Sulphuric acid, H2SO4, (strongest you can find)
Sodium hydroxide, NaOH (caustic soda)
Sea salt crystals
Distilled water (DH2O)
Give everything a good clean before start up.
Rinse the glassware with acetone.
Get hold of a PVC irrigation fitting that will reduce the gas bottle out let down to take the clear plastic hose.
Now stand the gas bottle in a tub of ice & water to chill. Or stick it in the freezer.
Get the coffee mug & fill it with Xylene.
Get the batteries & the tools.
Take your battery and break off the top:
If you are just beginning, the best thing to do now is peel that sticky label off enough where you can see what you are doing.
Now get something to grasp onto the "lip" and break it off.
You should come up with 4 little pieces (2 silver and 2 plastic rings)
Being careful not to let any metal stay in contact (tools touching the silver parts or crimping some together); start taking sections of the casing and start pulling away. If the battery begins to heat up and you can't find where anything is in contact, throw it in your mug so it won't ignite.
Take a pair of needle nose pliers and start rolling each section down like you were
"Peeling" a banana.
Keep doing this until you are able to completely remove the casing. On the side at the bottom there will be a silver strip. Completely remove it by getting a good grip and pulling it out.
Do not uncoil then just drop them in the coffee mug for later.
Warning on the storage of Lithium -
Using the wrong solvent (especially halogenated and protic solvents) can and will lead to fires and possible explosions. Safe solvents include dry toluene, xylene, pentane/hexane/heptane, as well as pure petroleum ether or naphta (if you are unsure about the purity, use something else!).
Get the pot and the Pyrex jug.
With the jug in the pot, pack the gap between them with dry ice then pore acetone onto the dry ice. There will be a bit of froth & bubble as the temperature equalizes.
Get the baking try and the shot glasses.
Put about 10mm of Xylene in the try, and then unroll the batteries. Find the end of the wrapping and start to unroll. It might be like a roll of tape getting started and try to strip into sections so be sure and get it to where it unrolls even. When you get it unrolled you will have a black layer, 2 white ones with a dull silver one in between them. This is your lithium and will start to heat up as it is exposed to air.
Lay the strips in the try & hold then under with the shot glasses.
Go & get the gas bottle out of the tub & give it a quick wipe dry.
Put it up side down next to the pot with the jug in it.
Now make shore all skin is covered, respirator on, gloves on & eyes protected.
With one hand hold the hose in the jug & put the other hand on the gas valve, slowly open the valve. Fill the jug up to the 250ml make printed on the side & shut the valve.
Put the gas bottle the right way up away from the work area, check the valve is closed.
OK, now the genie is out of the bottle so take care. If there is a splash & it gets on you, just poor some water on it. The most important thing to remember is don’t panic.
There is plenty of time so don’t rush.
Paper towel & stirring rod at the ready, brake a ¼ strip of lithium of, quickly pat dry with the paper towel & drop it in the ammonia, stir for 10 to 20 seconds then repeat until all the strips of lithium are dissolved.
Now go get the pseudo from that clean dry place that it is stored.
Slowly add the pseudo over about 10 min stirring vigorously.
Don’t add to quickly there is a big difference in temperature hear so allow it to equalize.
Give it a real good stir right at the end.
Remove the jug from the ice bath & stir for a further 10 min.
Allow the jug to stand for 15 min or so to let the ammonia evaporate.
When it’s almost all evaporated add about 100 ml of DH2O, (3 shot glasses).
There will be a bit of froth & bubble, after that add about 70 ml of toluene, (2 shot glasses). Give it a quick stir, and then let it stand & come up to room temperature.
Now add to the jug NaOH. ¼ teaspoon at a time & stir, keep doing this till on more bubbles come up from the water later.
Get one of the bottles, put the funnel in it. Hold the tee strainer over the funnel & pore the contents of the jug through the tee strainer down the funnel into the bottle.
Grab the bottle put a thumb over the top & give it a shake, like shaking up a can of spray paint.
Set up the separation funnel, make shore the tap is shut. Pore the contents of the bottle into the separation funnel.
Go wash out the Pyrex jug dry it & rinse with acetone, allow to dry then put 70 ml of toluene in the jug.
Go back to the separation funnel, put the jug under the sep funnel, let the water run out of the sep funnel into the jug, from the jug put it in the bottle & shake shake shake .
Pore the contents of the bottle into the separation funnel.
This is called pulling, getting the Meth out of the water onto the toluene.
Four (4) pulls will do. Repeat above steps.
Now there should be a separation funnel with about 300 ml of toluene in it.
On the side of the sep funnel there will be little squiggly lines of water between the glass & the toluene, get the stirring rod put it in through the top of the sep funnel & push the lines of water down to the bottom. Get all the water out.
(An optional extra is to dry the toluene with oven baked Epsom salt).
Grab the weed sprayer & pull it to bits. There will be assembly lubricants on the internal parts so wash everything with acetone.
Throw away the trigger gun and all metal parts.
Put the sprayer back together, but leave out the pressure relief valve just stick some paper in the hole & pinch it over with the pliers. We wont it to leek little. Also pinch down the end of the hose to make it smaller.
Clean out the Pyrex jug & rinse with acetone.
Put the 300 ml of toluene/Meth in the jug.
Put gloves & respirator on.
Open the top of the spryer, drop in about 500g of sea salt followed by (½) shot glass of H2SO4, and then (½) shot glass of HCI & putt the lid on the sprayer.
Gloves off, respirator stays on, pick up the sprayer & lightly slosh it around kind of like sloshing wine around in a wine glass, it should have the sound of the salt scratching lightly on the bottom. (Do not shake it up & down).
Put the end of the hose down in the bottom of the jug of toluene & pump the sprayer.
That white vapor is HCI gas it will tern the good stuff into a salt, that’s the white gunk that stating to show in the toluene.
After it had a good gassing, go get a coffee filter put it in the funnel, put the funnel in a clean bottle & pore the toluene trough the filter, and give it a good chance to drain.
Put the coffee filter with the stuff in it aside to dry.
Pore the toluene out of the bottle back into the jug, gas again & filter. Continue gassing & filtering until all that comes out is yellowy brown slime that means all the Meth has been recovered.
Wash & recrystalize.
This is the simplest version of the Alan variation of the Birch reduction.
The resulting salt is purified isomer d-Methamphetamine HCl.
The recrystallized isomer is commonly call "ICE".
Main side reaction is Lithium chloride witch is removed by polarization in the post reaction separation.
If you have a chemistry question regarding the process feel free to ask.
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