Example of isomer separation for Meth

[qwe111]

Dear Mr.
Use L tartaric acid to separate the free base according to your method.
I got a chewing gum-like substance while stirring, and once I stopped stirring everything turned into a very hard white solid. A whole piece.
Is this correct?

 

[btcboss2022]

Yes

 

[btcboss2022]

It won't turn liquid the liquid is mixed with the hard solid you must crush it to vacuum filtration and get the liquid.
About freebase yield from p2p is ok if not steam distilled p2p used.

 

[qwe111]

Dear Mr.

I used L tartaric acid to separate the free base. Vacuum gives liquid. Alkaline PH-13. Free base is obtained.

Stir the free base. Join HCI. PH value -2. I wanted to adjust the pH to -3. But the pH suddenly dropped. I'm careful to add very little HCI. The pH value has always been around 7 in the beginning. Then suddenly it drops to -2.

Heat to 130°. Pour into a container with 10 volumes of chilled isopropyl alcohol. A lot of powder immediately appeared in the container. Shouldn't we get crystals?

What did I do wrong?

Sir, please help me.

 

[novato]

The next step after the separation of the isomers would be to add sodium hydroxide dissolved in water, to the remaining tartaric acid, hydroxide is added until you reach ph13 and oil will be made, that oil will be cooked with thiol and percadox, in the following way or process.
To each 30 liters of oil 2 liters of thiol or thiol will be added, it will be boiled until it reaches 160 degrees centigrade, once you reach that temperature 2 kilos of percadox is added little by little because it will make a reaction, it is stirred so that all the percadox is dissolved and is homogeneous and the temperature is maintained for 10 minutes more.
Then it is left to cool at room temperature and the next day or once cooled it is added again tartaric as in the first process to separate the isomers and there the cycle that appears in the image.

 

[btcboss2022]

Hello,

What is the source of that info please?
Thanks.

 

[novato]

It has already been done, which is why the explanation is so detailed.

 

[btcboss2022]

I don't know the source of that process but adding perkadox at high temp has a big risk of explosion, in fact it shipping only could be done in special containers to have a temp below 20C and that's not to mention the difficulty in obtaining that product, which makes it necessary to be very sure about the process to try to obtain it.

 

[novato]

If you make a reaction at this temperature and that is what is conducive to the l isomer becoming d

 

[btcboss2022]

And whats the source of that process please?Thanks.

 

[btcboss2022]

And another important problem here is that Perkadox is a brand name and has many different products for initiators (Di(4-tert-butylcyclohexyl) peroxydicarbonate,AIBN, AMBN, ...)each one works different in amount and temperatures I guess that for that process Di(4-tert-butylcyclohexyl) peroxydicarbonate is used but AIBN could be used too in correct ratio.

 

[subzero]

Is it true that levo salts will start to pp if l-tartaric acid is added in excess ?

 

[Jorg]

We call it Netherlands ship method of recycle. Heard only good things about it,didnt try it out yet. Thanks for the post.

 

[hunter12]

Please help, after mixing amd leaving it overnight it turned out pink.

 

[btcboss2022]

Pink color normally means too acid but not in 100% of cases also could be impurities from your freebase, check the PH should be around 4 anyway I dont see any precipitate in your pic.

 

[hunter12]

I used clean distilled meth freebase. The PH is 4.5-5. There are no precipitate. And it only heat up to around 30 degrees during vigorous mixing. There was no precipitate that showed even during mixing

 

[btcboss2022]

Tell me all details if not can't know where is the possible problem.

 

[hunter12]

I mixed 160ml water and 70 grams tataric acid then added 100 grams distilled freebase with heavy stirring (using magnetic stirrer). It got aqueous cloudy but with no precipitate, then left it overnight and found it pink in the morning

 

[hunter12]

I used l-tartaric acid (cas 87-69-4)

 

[qwe111]

Is there some thick material appearing on the walls of the beaker during stirring?
If there is. Use a glass rod to scratch the side of the beaker. Will help with crystallization.

 

[btcboss2022]

Try 150ml h2O+80gr tartaric once dissolved add the freebase with heavy stirring until solid mass formed could take some minutes.

 

[hunter12]

Ok thanks il try that, il come back with results

 

[btcboss2022]

On my experience I think it needs more time stirring it's getting thick and finally solid.

 

[hunter12]

This is how it is