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.
need help converting 5449-12-7 and 20320-59-6
- Thread starter strangerdanger
- Start date
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.
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.
Hello,
what percentage concentration for hcl?
Thank tou
what percentage concentration for hcl?
Thank tou
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
what is the ph off your milk ?
if you follow my instructions step by step you had no milk
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this is the preparation of P2P Phenylacetone CAS 103-79-7 made use of BMK Glycidic Acid ( sodium salt ) CAS 5449-12-7 with main ingredient sulfonic acid strength is 75% CAS 7664-38-2
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we are going to prepare 1 kg of BMK
take a 5 liter double neck flask
add 500ml boiling water . start with the mixer.
now very slowly add 1kg of BMK salt. ( 30 minutes )
then add 1 liter of sulfonic acid.
and heat the contents of the flask to max temperature. plus minus 130°c. use a powerful mixer.
now connect the reflux
Let it boil in reflux for 4 hours.
take the top layer and pour it into a measuring cup.
let the bottom layer cool and save for next time. ( we have no chemical waste for this preparation method )
now boil 1 liter of water and add it to the measuring cup. use a hand mixer to mix everything.
After mixing for a few minutes, let the measuring cup cool to room temperature.
remove the top white layer (this is water and waste that we don't need)
the bottom layer is P2P purified and ready to use.
ps: in this preparation we don't have to worry about water remaining in our P2P because water weighs less than P2P
ps2: if you keep these ratios, the P2P will have a ph value of 4 .
if you use more sulfonic acid the ph value will drop to 1. Therefore it is not necessary to use too much sulfonic acid.
Which "sulfonic acid" did you use?
Sulfonic acids are a class of organic compounds which contain a sulfonic acid group (-SO3H) attached to a carbon. You sulfonate an aromatic compound to form a molecule which contains the sulfonic acid functional group. But to my knowledge no such thing as "sulfonic acid" exists.
Which aromatic compound did you sulfonate?
Can you provide a CAS number of what you're talking about? Your route sounds very interesting but it depends on the originating aromatic compound due to the price.
Or did you mean sulfuric acid (H2SO4)?
Sulfonic acids are a class of organic compounds which contain a sulfonic acid group (-SO3H) attached to a carbon. You sulfonate an aromatic compound to form a molecule which contains the sulfonic acid functional group. But to my knowledge no such thing as "sulfonic acid" exists.
Which aromatic compound did you sulfonate?
Can you provide a CAS number of what you're talking about? Your route sounds very interesting but it depends on the originating aromatic compound due to the price.
Or did you mean sulfuric acid (H2SO4)?
It's just a joke, sorry moderators if it's out of place. I was just making abit of fun of Saul who thinks people encourage the use of HCl for some nefarious or conspiratory reasons.
what is the problem of yields with 5449 coming out so low?
the most i get is 47.5% yield with phosphoric acid 75% or 35% with hcl 36%
does phosphoric acid have to be 85% to achieve yield in range from 60-70%?
or why does the ratio: 1kg bmk : 1.5L phosphoric acid : 0.5L water give out only 47.5% yield at the most?
did anyone of you have such experience?
could the bmk powder be of low quality or have something mixed in to not give so much yield out?
people with experience help @btcboss2022 @G.Patton @sponsor
the most i get is 47.5% yield with phosphoric acid 75% or 35% with hcl 36%
does phosphoric acid have to be 85% to achieve yield in range from 60-70%?
or why does the ratio: 1kg bmk : 1.5L phosphoric acid : 0.5L water give out only 47.5% yield at the most?
did anyone of you have such experience?
could the bmk powder be of low quality or have something mixed in to not give so much yield out?
people with experience help @btcboss2022 @G.Patton @sponsor
- By btcboss2022
Obviously we cant know if your 5449 is mixed or if Its good quality or not ;-)
In my case I always used phosphoric at 85% 1:1,2:0,5 powder, acid, water
You can try to make the process without H2O, Heat the acid around 60C and add the powder portionwise while stirring, once all added reflux 5 hours at 140C with slow stir.
In my case I always used phosphoric at 85% 1:1,2:0,5 powder, acid, water
You can try to make the process without H2O, Heat the acid around 60C and add the powder portionwise while stirring, once all added reflux 5 hours at 140C with slow stir.
- By G.Patton
Agree with @btcboss2022 . You have to check mp of you BMK glycidate at first. How did you calculate reaction yield?
@G.Patton and @btcboss2022 thanks both for answers, it is weird because supplier says it is 100% 5449
I did not try melting point of my bmk glycidate, I calculated reaction yield on the proportion if from 200g of powder comes out 90ml it means 45% yield
but it is probably wrong calculation because i did not use moles of reactants
could this powder be diethyl phenylacetyl malonate? and this is why such small yields? or was the diethyl phenylacetyl malonate only available in oily form?
I did not try melting point of my bmk glycidate, I calculated reaction yield on the proportion if from 200g of powder comes out 90ml it means 45% yield
but it is probably wrong calculation because i did not use moles of reactants
could this powder be diethyl phenylacetyl malonate? and this is why such small yields? or was the diethyl phenylacetyl malonate only available in oily form?
- By btcboss2022
20320 has powder form too but I dont think that method works for It are different productos.
- By G.Patton
Read this manual to count the yield correctly. Moles, grams, liters and chemical calculations
You had to get 132.7 ml of P2P from 200g of 5449-12-7. You've got 67.8% yield. Do you feel difference with your 45%?
You can check melting point of your precursor 5449-12-7. If the melting point will be different more than ~5 deg C, your product is polluted. I don't thinks that problem is there.
You had to get 132.7 ml of P2P from 200g of 5449-12-7. You've got 67.8% yield. Do you feel difference with your 45%?
You can check melting point of your precursor 5449-12-7. If the melting point will be different more than ~5 deg C, your product is polluted. I don't thinks that problem is there.
@G.Patton thanks again for answers but i think you calculated it wrong, the best yield i got is 95ml yellow oil (p2p) from 200g powder, so how much yield is this? not 67.8% i think.... it is way less or? i just dont understand how to calculate this yield and i've read that moles,grams, liters and chemical calculations thread you posted here
this is a normal amount p2p
the next stage is more important
and the last stage is the biggest secret off the forum
the next stage is more important
and the last stage is the biggest secret off the forum
- By G.Patton
Read my post about calculation again, there is paragraph How to calculate yield. If you don't understand, ask there.
>the best yield i got is 95ml yellow oil (p2p) from 200g powder, so how much yield is this? not 67.8% i think
you think wrong.
200 g Of glycidate is ~1 mole (0.999167479). According to reaction balance, you have to get 1 mole of P2P. 0.9991674 mole of P2P is =0.999167x134.18g/mole=134.07 g. Volume of 134.07g P2P is 134.068g÷1.01g/ml=132.74 ml. You've got 95 ml. The yield is = (90 ml*100)/132.74 ml = 67.8%.
>the best yield i got is 95ml yellow oil (p2p) from 200g powder, so how much yield is this? not 67.8% i think
you think wrong.
200 g Of glycidate is ~1 mole (0.999167479). According to reaction balance, you have to get 1 mole of P2P. 0.9991674 mole of P2P is =0.999167x134.18g/mole=134.07 g. Volume of 134.07g P2P is 134.068g÷1.01g/ml=132.74 ml. You've got 95 ml. The yield is = (90 ml*100)/132.74 ml = 67.8%.