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

[btcboss2022]

In your picture above, there seems to be 3 layers, first one yellow transparent, then in the middle dark layer and then on the bottom also yellow layer
Or am I not looking at it properly?

So normal steal distillation can be used for p2p? It will boil over with water?

ChingShihTheres not a yellow transparent layer is the colour of the bath fluid in the jacketed reactor.
Normal steaming can be used for P2P boiling with water.

 

[Bartholomeus]

Theres not a yellow transparent layer is the colour of the bath fluid in the jacketed reactor.
Normal steaming can be used for P2P boiling with water.

btcboss2022
Thanks for all the answers

 

[Saul]

Theres not a yellow transparent layer is the colour of the bath fluid in the jacketed reactor.
Normal steaming can be used for P2P boiling with water.

btcboss2022
I also dont understand this picture ? there are 3 layers what is that black layer ?

 

[Saul]

so just to be clear.
after 5 hours of cooking, let everything cool down.
then you take the top layer and keep it separate.
what's the next thing you do with the top layer?
And what do you do with the bottom layer?

I want to become A-oil

 

[Saul]

at 5449-12-7

1 kg ap 0.5 water 1.2 phorsphor
140 degrees 5 hours with agitator
You have to get 140 degrees at a lower temperature you get dirty oil

Brombeer88this is making more sence !
phosphoric acid boiling point is 158°c so you can get with no problem 145°c ( you have it right )
Formic acid 83% boiling point 100,8 °c ( not possible to get more than 110°c )
Hydrochloric acid 30% boiling point 90 °c ( useless ! ! )
Hydrochloric acid 37% boiling point 50 °c ( useless ! ! )
Sulfuric acid 96% boiling point 337 °c

next time you laugh at someone think twice .
you know who you are ( not at brombeer )

 

[btcboss2022]

I also dont understand this picture ? there are 3 layers what is that black layer ?

Saul2 layers the black one is the oil.

 

[btcboss2022]

so just to be clear.
after 5 hours of cooking, let everything cool down.
then you take the top layer and keep it separate.
what's the next thing you do with the top layer?
And what do you do with the bottom layer?

I want to become A-oil

SaulTop layer could be purified or not depend what you want to do with it for A oil possibly not interesting to purify it.
Bottom layer is discarded but you can extract it.

 

[Bartholomeus]

Top layer could be purified or not depend what you want to do with it for A oil possibly not interesting to purify it.
Bottom layer is discarded but you can extract it.

btcboss2022
But wouldn't dirty oil reduce the yield on a reductive amination of p2p to amine?
Wouldn't be better to purify and then make leuckart of that pure p2p, so less impurities comes in final product...
But the user broomber88 is having quite good yield from everything as he wrote

 

[btcboss2022]

I did that conversion in large scale more than 5 times and temp of the mixture don't goes higher than 120C even you put reactor temp at 170C should be refluxing products don't get more temp than this it happens many times in different reactions.

btcboss2022I 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]

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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btcboss2022Hi 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]

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?

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

 

[Jordan Belfort]

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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btcboss2022That'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.

 

[Bartholomeus]

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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btcboss2022
Thanks for the update, it helps a lot for us others to learn
@btcboss2022 please if you can reply to my question for you in the Nabh4/Cucl2 P2NP thread

 

[btcboss2022]

Thanks for the update, it helps a lot for us others to learn
@btcboss2022 please if you can reply to my question for you in the Nabh4/Cucl2 P2NP thread

ChingShihWhat question do you mean? I don't see it.
Thanks.

 

[Bartholomeus]

What question do you mean? I don't see it.
Thanks.

btcboss2022
Please look at the last page (6.page) of thread: One-pot synthesis of amphetamine from P2NP with NaBH4/CuCl2 (1kg scale)
On 12th of July I posted few questions for you @btcboss2022 and for @William Dampier because you two have experiences with this reaction
When you have time please answer to those questions as it would help me very much

 

[Wizzkid]

Hello again,

Ok I tested with phosphoric acid and is a cheaper synth because less product must be used and possibly shorter too:


BMK powder(CAS 5449-12-7)1Kg: H2O 0,5 liter: Phosphoric acid 85% 1,2 liters

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

120C reflux at least 3 hours( I did it 5 hours and no difference with final result)

With 20kg of powder I obtained 13 liters of "dirty" oil that must be purified or not depend the final use.

The aquos phase could be extracted with DCM but I did it and not enough product to this long job but each one can decide.

;-)

btcboss2022Could 75% phosphoric be used at the same ratios or would this need 85% ? Just easier to get hold of currently

 

[G.Patton]

Could 75% phosphoric be used at the same ratios or would this need 85% ? Just easier to get hold of currently

WizzkidYes, you can. But you have to take more acid. 1.2L of 85% = 1.36L of 75%

 

[Saul]

Yes, you can. But you have to take more acid. 1.2L of 85% = 1.36L of 75%

G.Patton
dear mr Patton,
is it possible to transfer phosphoric acid 75% strong to 85% strong?
becouse 75% is verry easy to get and cheep to

 

[btcboss2022]

Not necessary you only need to add 10% more of product than 85%

dear mr Patton,
is it possible to transfer phosphoric acid 75% strong to 85% strong?
becouse 75% is verry easy to get and cheep to

Saul

 

[Saul]

Not necessary you only need to add 10% more of product than 85%

btcboss2022
thx you

 

[Saul]

Today I finally give it a try

 

[Wizzkid]

after steam cleaning the A oil the oil has become more acidic. I’ve put in caustic again but it’s gone dirty again (not as much as before but noticeably more than it was). Is there a better way to correct this ? Should I give the water a higher ph before distilling or any other tips ?

 

[btcboss2022]

Hello again,

After having some problems with the temp of the phosphoric route I decided to make small scale to test the traditional synth for BMK glycidate with HCL.

BMK 5449:H2O:HCL(37%) 1:1:3

- Solve the powder in hot water
- Add the HCL and reflux 5 hours with stirring(you can stop stirring at 2 hours for example and if it's still powder undissolved in the bottom you can add more water)
- Separate the 2 layers, wash with water the oily layer and separate it.
- Add DCM to the water layer and separate it.
- Add the separated DCM to the oily layer keep it before.
- Add anhydrous sodium sulfate to the mixture, stir and filter it.
- Evaporate the DCM.
- Now you have clean B-oil!