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

[strangerdanger]

been trying to convert both of these CAS to p2p without any luck. Ive attempted many different recipes for each and still no luck.

i doubt its the product as i have different samples from different suppliers and end up with the same.

willing to donate XMR for help with successful conversion

 

[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]

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.

btcboss2022Dont basify at start

 

[btcboss2022]

Dont basify at start

edyvanellende?

 

[strangerdanger]

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.

btcboss2022
NICE. Sent you PM

 

[btcboss2022]

Hello,

For CAS 5449-12-7 I did the official process of 1:3hcl refluxing 5 hours and it don't works properly very low yield and solid residue produced we made it 2 times we will add some changes and update you.

 

[strangerdanger]

Hello,

For CAS 5449-12-7 I did the official process of 1:3hcl refluxing 5 hours and it don't works properly very low yield and solid residue produced we made it 2 times we will add some changes and update you

btcboss2022Thanks for the update. I sent you a private message couple days ago

 

[Saul]

Thanks for the update. I sent you a private message couple days ago

strangerdanger
hello , plz dont sent it private . this is a forum to help others to just share it here so other people
can start from this and even improove it

 

[btcboss2022]

We changed 2 parts oh HCL for 2 parts o acetic acid without many changes.

 

[Bertusbats]

Succes?

We changed 2 parts oh HCL for 2 parts o acetic acid without many changes

btcboss2022

 

[Selassi]

Did u try phosphoric acid?

 

[Selassi]

1:1,5L not kg

 

[btcboss2022]

Succes?

BertusbatsHello 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.

 

[kwisspeed de Kelog's]

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.

btcboss2022Hello,
what percentage concentration for hcl?
Thank tou

 

[btcboss2022]

Hello,
what percentage concentration for hcl?
Thank tou

kwisspeed de Kelog's37%

 

[kwisspeed de Kelog's]

37%

btcboss2022Thank you

 

[hustlerkid]

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.

btcboss2022HCl is determined to give best yield?

 

[Selassi]

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.

btcboss2022Have u made any progress on the 5449?
What was the yield?

 

[Saul]

dont get it 5449 is easy to buy but nobody can transfer it to pgp

 

[Saul]

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.

btcboss2022
you had explane step by step someware but I not can find it and what is HCL zoutzuur ?

 

[Selassi]

HCl is hydrochloric acid, also known as zoutzuur indeed

 

[Saul]

HCl is hydrochloric acid, also known as zoutzuur indeed

Selassi
there is only 30% pure this means there is 70% water in it so the amount off water use for this synthesis is lower I guess?
is this also the one he use here ?

 

[Saul]

I think 300 ml water is enoug if HCI 30% is use .
is this possible ?

 

[Selassi]

Yes HCl 37% is mostly used in conversions. If u use water or.not depends on the recipe needed with the specified CAS

But there are many ways for this conversion

 

[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.

;-)

 

[Bartholomeus]

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
Do you thing using 2.4 liters Phosphoric acid 85% would give out more yield?
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?