need help converting 5449-12-7 and 20320-59-6

[btcboss2022]

I had success with 20320-59-6 liquid form but not with 5449-12-7 powder yet but I will get it for sure ;-) making some tests now.

 

[edy's]

Dont basify at start

 

[btcboss2022]

?

 

[btcboss2022]

Hello I tested many ways and the best yield with HCL is:

BMK powder 1Kg: H2O 1 liter: HCL 3 liters

Better dissolve the powder stirring in the hot H2O and later add the HCL

90C reflux at least 5 hours.

I will test phosphoric method soon and update you.

 

[hustlerkid]

HCl is determined to give best yield?

 

[Bartholomeus]

So the obtained oil after conversion from bmk powder can be used straight to leuckart or other reduction methods?
What do you think is the highest % yield reduction method from p2p to amph?

 

[edy's]

Look for the TOLMY script on www its an ausi hwho put his script on the web,youll love it

 

[whersiet]

ToLMY?? where am i looking for the acript

 

[Saul]

Hello my friend,
Is it possible that you make a new final topic off your conversion 5449-12-7
becouse so many wrong information on 25 different topics

it is realy shit that we can not edit topics here on braking bad
it makes no sense at al .
it could be so easy and clear if you could change the text after improved synthesis .
becouse off this it is almost impossible to find the right information the first time. 25 topics from 5449-12-7

I also dare to say that it is very dangerous not to be able to edit. in chemistry improvements are found every day.
Replacing heavy chemical products with less harmful ones seems to me to be progress.
but here on breaking bad the wrong harmfull information stay online for life
becouse the original post can not be edit after a new much better synthesis

 

[Gale]

There is a reason they lock your ability to edit.

Many other sites do the same thing, once you post, it becomes property of the forum lol useful when people delete info

 

[whersiet]

What other sites/forums is there like this ome?

 

[Bartholomeus]

Take 5 Liter or 10 Liter Flask

Step 1. Put 1kg bmk powder in flask, add in 0.5 Liter boiling water, start stirring the mixture, after dissolving, add 1.2 Liter Phosphoric acid 85%
Step 2. Bring this mixture to 140 degrees celsius, then boil for 5 hours with stirring
Step 3. After 5 hours of boiling stop the stirrer and heating and let the oil separate from mixture
Step 4. Decant the oil that is separated from reaction mixture and use it directly to further reductive amination methods to obtain A oil

 

[MCstojan]

If I have 20320-59-6 Oil is it the same procedure?

​

 

[Tweaker]

Do you need to adjust the ph before further processing?

 

[btcboss2022]

Middle layer? There are only 2 layers and the oil is the top one.
Yes around 11 liters:
- Steam distillation.
- Separate oil from water layer.
- Extract water phase with DCM.
- Dry with sodium sulfate and filter it.
- Evaporate DCM.

 

[rothschild33]

Will vacuum distillation work for the top layer instead of steam distillation?

 

[btcboss2022]

Aoil boiling point is 200-203C if you have enough vacuum power to achieve that temp without passing 60C is possible.

 

[btcboss2022]

Oh sorry I see now that are you asking about p2p right?So many different posts sometimes I get crazy hahaha P2P could be distilled with vacuum no problem boiling point is 216C make your maths with your vacuum power ;-)

 

[Jordan Belfort]

if you heat p2p over 145/150 it start's smoking.

moment it starts to smoke you slowly kill/destroy the oil.


Last time with vacuum distill I put oil bath to 210 but my reactor had no blanket on. because of that the oil condesned back (was outside) and partially burned because of that.

Was d-meth oil according to high and the smell.

 

[Jordan Belfort]

How you get higher vacuum then 1 bar, which small pump you use ?

I cannot get past little over 1 with two pumps in serie (stage one and vevor)

 

[btcboss2022]

I don't use a small one I use a big one. But I don't distill P2P at vacuum normally.

 

[Jordan Belfort]

What solvent on 1L, becuase baking soda is not very soluble in water unlike natrium chloride?

 

[btcboss2022]

I use water

 

[btcboss2022]

I uploaded some videos about process with phosphoric and as you can see mixture temp don't get higher even I put the reactor temp very high.
After around 3 hours you will see the oil mixed in the mixture. I got 14 liters from 20kg of powder.
When stop stirring layers get separated, aqueous layer discarted and I add water to wash the oil from acid.
Water layer discarded again and this "dirty" oil could be used in other processes.
Yield from "dirty" oil in meth oil process from example:
From 966gr of B oil I got 800gr of meth oil.

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[Heisenblack]

Hi btcboss2022, is it possible that you can re-upload/share these videos if you still have them?
Also, did you use reductive amination via Al/Hg to obtain the 800gr meth oil from B-oil?

 

[btcboss2022]

I dont have these videos sorry and I didnt use It Al/Hg router sorry too.

 

[Jordan Belfort]

That's really high, it was CAS 5449 ?

I also had problems with phosphoric acid. I wanted to do sulfuric acid way again because that way is NEVER headache.

I turned with phoshoric acid, small test on 5L engelmeyer no problem oil was day next really thin.
Second one I did oil wasn't as thin but was clear (means no good turning)

Then the other 2 where cloudy.

Now I heard from other people they do 1L phosphoric acid, 1KG 5449 and 1L of water but don't turn for 5-6 hours but up to 9 hours.
Then if they make a-oil the end product is 58L supposably the same as with sulfuric acid.

 

[Sjeik]

1kg bmk, 1.7-1.8L 85% phosforic acid,
4-5h cooking 130/140’ after finishing put 0.5L h2O let it cool down And it Will seperate.

 

[Heisenblack]

Hi Sjeik, what was your B-Oil yield from 1Kg BMK?
After finishing, is the 0.5L H2O just pure distilled H20 or brine solution?
Lastly, what temperature should the H20 be?

 

[btcboss2022]

I read some comments about the reuse of the phosphoric acid after a process please dont do it, even solvent extraction made to "clean" the acid you only will obtain a very strange semi P2P intermidiate product so dont waste your time on it and waste tour money in new acid.
The unique way would be distilling the acid at 158C but I dont recommend you.

 

[Jordan Belfort]

I can confirm, use the phosphorus waste from 5449 to convert p powder.

You can also reuse 3 times of you let the foam reaction of 5449 in a bucket and then suck the half converted oil into glas and then 150 celcius 12 hours and then do the pmk neutralize with Cs and p powder.

Also dont clean your b good so you have traces of meth in your Molly. Its really good molly then