Need help convert bmk 5449-12-7 to free base A-oil

[Saul]

today I try again.
after boiling with HCl for two hours, I separate layers.
keep the black layer and basified to ph14 keep it mix for an hour .
then leth it rest for 6 hours and remove the water layer .
after this I add toluene to the black layer but no layers form
and product destroyed.
toluene smells exactly like thinner

 

[tibby328]

Your lying , i can put money on it the maximum yield is 50 oercent from the leuckart.

 

[melk]

if you do it the long time way you get allot more than 50% ( info from PDF files )
when you mix mierenzuur + ammonium formate to an nice pH off 7 you get ammonium carbonate
and then add your p2p to the carbonate
and let it room temp for seven days, you get allot more yield .

 

[UWe9o12jkied91d]

In 1 mL scale with the help of heat and microwaves it is done in 1 minute with 90+ yields.I don't think anybody tried to scale it up, but would be cool

 

[Bartholomeus]

after 4 hours of boiling i got back yellow oil on top
i let it cool down and next day separated it and added boiling water to it 2 times to wash it
after the washing the oil became light yellow milky color
and the yield was very bad (40% - 200ml from 500g 5449)
at first i tried to add only 250ml water and 500g bmk powder but the bmk didn't dissolve and started to burn a bit so i added another 250ml water
and then the bmk finally dissolved

why is the oil now milk color? why is it not light yellow color like it was when it was converted?
and why was the yield so small? because of too much water added?
please guys share your experiences what it might be

 

[sponsor]

so you wa
so you want to make P2P from BMK salts?
what do you use for chemicals?
HCl does not work!
I know it's all over the forum, but it doesn't work at all
you need a chemical with a much higher boiling point for good yields
and use enouch water to start with becouse
the water evaporates first because the boiling point is lower
you need to start reflux when the temp is higher than 130°c
then you know the water is gone and then you boil in reflux for 3 hours

 

[Heisenblack]

Hi sponsor, so water is really not necessary? Can one start by adding the BMK salt to warm/hot acid and starting the reflux?

 

[Bartholomeus]

Sorry forgot to add this:

''cas 5449-12-7 has been tested on following procedure:
500g water, 500g bmk and 700ml phosphoric acid 75%''

And the pictures is what i got out of... so i did something wrong but now only question is what?

 

[Bartholomeus]

@sponsor

so you first boil the water, add the bmk powder slowly to dissolve, then add the phosphoric acid
and then boil the reaction without condenser on top until temperature of 130C is reached
and only then put the condenser on top and make reflux for 4 hours?
is this what i wrote now correct?

 

[sponsor]

.

 

[sponsor]

yes it is

 

[Bartholomeus]

thanks very much for answer
i probably made mistake, because i dumped the whole bmk powder in cold water inside flask
then it didn't dissolve and then i had to pour water again
i will try the recipe that is posted here again with proportions: 250ml water, 500g bmk and 700ml phosphoric acid 75%
this has to work

 

[sponsor]

boil the water start mixer and add slowly the bmk take your time for this

500ml phosphoric acid 75% is enough for 500gr bmk

 

[tibby328]

Mate you dont have a clue what you are talking about. If even if you could do that, ammoina carbonate is otc and very cheap. Let me know where you can can buy ammonia formate ok.
I dont think anyone on this site has a clue what they are talking about

 

[tibby328]

I dont think anyone on this site has a clue what they are talking aboutq

 

[Bartholomeus]

Instead of saying everyone here doesn't have a clue about what they talk then please enlighten us with your knowledge

 

[tibby328]

You are ok, theres are to many people on this site who want spoon feeding, and alot more posting wrong techniques. I will save my knowledge for the real forum

 

[tibby328]

If you need help private message me

 

[tibby328]

Sorry i sholdnt of said that my bad

 

[tibby328]

My Bad

 

[h20]

you also have no clue idiot !
otherwise you didn't ask where you can buy ammonium carbonate

 

[edy's]

Bakery supply store .caled bakers ammonium