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

btcboss2022

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Do you thing using 2.4 liters Phosphoric acid 85% would give out more yield?MOre
Did you basify (adding 50% Naoh) to the obtained oil after reaction?
Would you need to use vacuum for purifying that ''dirty'' oil?
Or normal steam distillation work?
ChingShihIn that case more acid won't increase the yield.
I don't basify the oil layer is separated.
About purication you can choose the method that you prefer don't affect final product.
 

Bartholomeus

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In that case more acid won't increase the yield.
I don't basify the oil layer is separated.
About purication you can choose the method that you prefer don't affect final product.
btcboss2022
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

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

Selassi

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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?
ChingShihYes can be used directly for further processing
 

btcboss2022

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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?
ChingShihHello,

Obviously the best yield of amph from P2P is converting it in A-Oil(Amphetamine freebase) and make the sulfate from it.
From a good A-oil you can get 2.8kg until 3kg of amph sulfate ;-)
 

Bartholomeus

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Hello,

Obviously the best yield of amph from P2P is converting it in A-Oil(Amphetamine freebase) and make the sulfate from it.
From a good A-oil you can get 2.8kg until 3kg of amph sulfate ;-)
btcboss2022
Sorry you understood my question wrong, I was asking what gives the most yield % - reductive amination method from p2p to amphetamine?
Other than Al/Hg or Leuckart Wallach ?
 

Brombeer88

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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.

;-)
btcboss2022
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.

;-)
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
 

Bartholomeus

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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
Brombeer88
Did you try this conversion?
Is 140 degrees your self-experiment results that makes purer oil?
What was your yield of oil from 1kg of bmk powder?
 

btcboss2022

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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
Brombeer88I 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.
 

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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.
btcboss2022
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

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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
SaulThere 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

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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
GaleWhat other sites/forums is there like this ome?
 

Brombeer88

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Did you try this conversion?
Is 140 degrees your self-experiment results that makes purer oil?
What was your yield of oil from 1kg of bmk powder?
ChingShihgood morning I did 5449 myself we use 1000 liter boiler with agitator do 250 kg ap 125 lt water 300 phorsphor acid
5 hours cooking at 140 degrees
175 p2p comes out then further on leucart reaction and we get 130 lt a oil from it so 52 liters a oil per 100 kg
 

Brombeer88

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good morning I did 5449 myself we use 1000 liter boiler with agitator do 250 kg ap 125 lt water 300 phorsphor acid
5 hours cooking at 140 degrees
175 p2p comes out then further on leucart reaction and we get 130 lt a oil from it so 52 liters a oil per 100 kg
Brombeer88you can come to the Netherlands and I'll show you
 

Saul

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you can come to the Netherlands and I'll show you
Brombeer88I am willing to make a donation for a step by step explanation for this 5449-12-7 inclusive which products you use and which hardware glass you use
for small scale let's say 1kg bmk

I ask this becouse I have to order all products needed to become A-oil
 

Bartholomeus

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I am willing to make a donation for a step by step explanation for this 5449-12-7 inclusive which products you use and which hardware glass you use
for small scale let's say 1kg bmk

I ask this becouse I have to order all products needed to become A-oil
Saul
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

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

 

Tweaker

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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
BartholomeusDo you need to adjust the ph before further processing?
 

Bartholomeus

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good morning I did 5449 myself we use 1000 liter boiler with agitator do 250 kg ap 125 lt water 300 phorsphor acid
5 hours cooking at 140 degrees
175 p2p comes out then further on leucart reaction and we get 130 lt a oil from it so 52 liters a oil per 100 kg
Brombeer88
Thank you for this answer, I sent you PM
 

btcboss2022

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you can come to the Netherlands and I'll show you
Brombeer88I trust you of course but I only can ask about my experience I will make pics about temp in the next batch, I put the temp reactor to 200C and the mixture don't get higher than 120C
Thanks.
 

btcboss2022

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Ib3Tx59jS0


This pic was from one of the past batches done with 20kg of powder during 3 hours at 120C.
The 14 liters "dirty" oil were purified and I obtained the 80% of pure and clean P2P.
I will upload the details of the next batch.
 

Bartholomeus

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View attachment 5759

This pic was from one of the past batches done with 20kg of powder during 3 hours at 120C.
The 14 liters "dirty" oil were purified and I obtained the 80% of pure and clean P2P.
I will upload the details of the next batch.
btcboss2022
Thanks for picture, the ''dirty'' oil is the middle layer - that ''black - brown layer'' of oil?
And what is the first and last layer? Why is the oil on the middle and not in the upper or downer layer?
I thought with this conversion only two layers form?
From 14 liters of dirty oil, you obtained like 11.2 liters of pure and clean P2P right?
What was your method of cleaning? Which type of destillation?
 

btcboss2022

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Thanks for picture, the ''dirty'' oil is the middle layer - that ''black - brown layer'' of oil?
And what is the first and last layer? Why is the oil on the middle and not in the upper or downer layer?
I thought with this conversion only two layers form?
From 14 liters of dirty oil, you obtained like 11.2 liters of pure and clean P2P right?
What was your method of cleaning? Which type of destillation?
ChingShihMiddle 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

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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.
btcboss2022Will vacuum distillation work for the top layer instead of steam distillation?
 
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Bartholomeus

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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.
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?
 
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