06-21-04 04:48
No 514512
Goodmorning all,.
You know, if you really want something, there is always a way,....
First of all, there are many analogues of codeine, many, many ,many,.
What we first have to do is create our tools to cleave and add fucntional groups, predominately acetyl, and methyl's to codeine.
Literature states that there are a vast range of tools to do this, all having their characteristic yields, If you look hard enough you will see that you can demethylate codeine in Koh, naoh,Hbr,HI, and the list goes on,.
But there has been alot of misconception over the fragility of the oxygen bridge,.
After reading many patents, I can see that this Oxygen bridge is tougher than we first thought,.
But just so we set about this journey the correct way, with yield our primary concern, we will closely follow proven patent results,.
The two tools we need to construct are Acetic Anhydride, and Boron Trihalide(your choice),.
These seem to be the pick of the crop for yield,.
About 9 months ago swim began researching this, and now it is my gift for you all,.
Acetic Anhydide - ---------------------------
Sodium Acetate....
1 litre of white vinegar( clear) is dumped into a large pyrex pot 5 litre capacity(coffee perculator), and sodium bi-carb is added and stirred till no fizzing is evident,.
It is advantagoues to leave the solution slightly acidic, as the base remaining tends to make clean up that bit harder,.
Any way, the pot is blasted on the stove, on high heat until the solution dries up, and looks a bit like Wheat-bix.,There are alot of impurities in here, but also a substancial amount of Na-acetate.
I think most people fail here because of a lack of otc purification solvent,
Well it's no secret, its ethanol, aka Methylated spirits.
To the hardrend crust remaining in pot, you about twice the amount of etoh,(enough when heated to dissolve all the sludge) and heat until all goes into solution.
Once this is done, you boil the liquid down to a point where you see it just start to solidify, take it of the stove, and leave to air cool, then right in the fridge,.
After about 20 mins, you will see a wonderful thing, shiny clear crystals forming inside the etoh solution, leaving behind the shit you don't want,.
You see that na-acetate is moderatly soluable in water, and a lot less in etoh, so with these two solvents, you can obtain perfect pure crystals, with no distillation.
You roughly get about 50-100g per 2 litres of vinegar,.
You repeat the process of warming the crystals in etoh, and ditching the remaing solution material,.(Swim doesn't he keeps it all, to get more and more crystals out of it,.)
Acetic Anhydride.
An aparatus is set up for the production of chlorine,
Swim used a collection a glass testubes, rb flasks, and teflon tape to make this happen, do not use plastic, as it will just fuk up eventually,.
So dump your bleach into the flask, add your hcl, at a rate that gives you a good flow, always use a water trap, otherwise hcl vapours will fuk it,.
Now, the chlorine generator is connected to the ignition tube(pyrex testube) which contains the sulphur (otc) and your fused(heated to remove moisture) na-acetate.(Cheers Rhod's, could never of done this without your page,.)
You do not have to heat the sulfur into a molten state, so this can be more or less one anywhere,
Chlorine freaks me out so swim spent about two weeks making a fume cupboard,(highly recommended)
As the chlorine is pumped into the sulfur and Na-aceteate misture, eventually it slowly turns to liquid, which is the Acetic anhydide forming, Once you are happy, that no more chlorine in being absorbed, the reaction is finished,.
Work out the amounts of chlorine you need first of all, and make your system out put that amount of cl2.
This foul greeny red vicous/solid is distilled initially with kno4 to remove sulfurous compound, and then redistilled to give you a good yield of this pungent yellowy stuff(acetic anhydride)
Bottle this, and keep it in freezer.
Boron Halides
Swim prefers Bcl3, as it is a gas at room temperature, you will find out why in a second.
It took swim about a week to get this into a reliable working proceedure, as All he had to follow were old patents,.
This is where it gets really interesting.....,ready?
We need a source of boron obviuosly, so if we look around we find out that borax, is the easist to obtain, then boric acid,.Boric acid is a welding flux commonly sold at hardware stores, but sometimnes it is mixed with impurities, so it is probably easier to just start from borax,.
Borax is fucking cheap, non suspiciuos and common, so..
46 g borax is dissolved in the smallest amount possible of water, 20.3 mls of Conc. HCL is added
The mixture is then cooled down, and filtered,
Hey you've just made boric acid, well done!
To purify it just dissolve again in the smallest amount possible of hot water, cool again in ice bath, filter.
Then another wash with etoh, will give you pure boric acid.
44% (13.2g)
Na2[B4O5(OH)4].8H2O + 2Hcl----> 4H3BO3 +2NaCl + 5H2O
(sweet)
And have a guess what happens when you heat this baby, well,,its..Its,......Boric Oxide( aka Boric anhydride)B2o3
So in RBF dump 25 g Boric Acid, heat at 300c for one hour
to leave 14.7 g of Boric oxide,.
So i hear you all say, why all this for Boric Oxide,
Well my friends, it's all inside patent 832,096 LONDON.
Which tells of the improvements made in the prep, of boron halides, Whoooh!.
Now for all intensive purposes, swim wants a gas to be the final product, so swim chose BCl3,.
Now there is a bit of a twist here, we are going to store the resulting gas inside Chloroform, at a certain molar ratio to de-methylate codeine,.
In a porcelin vessel, with a hole at the top, is placed Sodium chloride(salt) and Boric oxide, on a 1:3 ratio.
The hole at the top of the otherwise sealed ceramic vessel, is where you connect a thick pyrex tube, which leads out into chloroform, the tube is made long enough to considerably cool the gas before it comes into contact with chloroform,.
Initially you weigh your chloroform, and calculate a target weight, to give you the molar strength to de-methylate codeine,.
Swim used Mapp gas(acetylene/propane) to heat the mixture to the point where Nacl melted, About 800c.,.
Boric ocide melts at ~450c, so the trick to this to continuosly agitate the two molten liquid,.
Boron trichloride begins to emerge at around 800C, and this is carried, cooled, and bubbled through chloroform,.
Walah!
So you now have Acetic anhydide, and demethylating amount of Bcl3 in Chloroform,.
And that is it,.
The rest of the chemistry is straight forward, and you now have the arsenal to acetylate, and demethylate,
How dandy!
hoff
And if you really want I can get some pictures, as it is a beautiful and truly exotic reaction,
Some people say the war is over, and the doors are fully open, I guess this is just a reminder that anything is possible,.
Now, because swim does not like using chlorine, and bromine is out of the question, he is wondering is there would be someway to use hypochlorite in-situ with the na-acetate and sulfur,
If there are chemists here that now this,then Swim will never having to worry about cl production, which is deadly, and inconvenient to use,
anyway, good luck to all,.
hoffman
(Hive Bee)
06-21-04 06:38
No 514532
And if you really want I can get some pictures, as it is a beautiful and truly exotic reaction
Would be nice.
Can someone varify this method and proceedure?
-AC
Its just my opinion, but no-one listens to me anyway, and rightly so...
(Hive Addict)
06-21-04 06:54
No 514538
Everything's backed up by procedures that can be found on Rh's page or in patents. I hope you're prepared for the daemon.
I like the BCl3 preparation part, wanted to get into this for a long time.
--psyloxy--
itch me to death
06-21-04 07:00
(Rated as: incomprehensible)
06-21-04 07:09
(Rated as: insignificant)