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

Saul

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This weekend, I try again. This time I make my ammonium formate on front and let it boil a wile so the water is gone
and then I put it in the freezer and after that I use vacuum to dry it. So I know there is absolutely no water inside

What I don't understand is that so many people here claim to have succeeded in the synthesis.
but they don't post proof. I'm sorry but for me you failed.
 
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Bartholomeus

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Can you please explain how did you achieve this yield?
And what ratios of p2p and other reagents did you use?
 

tweaker2

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i think your problem is the p2p the conversion was incomplete did you only boil the bmk powder in acid?what is the ph of your p2p and how does it smell?pure p2p has very pleasant flowery smell
 
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I I have had APAAN that Had a very similar smell to bananas Wons converted to P to P has anyone heard this before?
 

KokosDreams

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Do you mean P2NP?

P2NP smells like marzipan and a little fruity too
 

KokosDreams

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Hmm, do you got a picture?

P2NP looks like this (attachement):

ASEIfmoFxi
 

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No it was lighter in color and was waxy to the touch but was also Crystal kind of shine to it if you get me will try get pic tomorrow
 

studentt

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hello,

i put 5kg powder 5l water and 5l hci. everything turned green. is that normal?
when i reached 3l hci i saw the oil. but i read more hci? is needed
 

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Saul

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I realy dont get it why people wanna use HCI for this .
if you can avoid HCI 1 good advice do it . boiling point is allot to low and most importand
you die from those gases. this is the worst product to work with.
you need to find you a chemical with boiling point minimum 140°c
AND ALWAYS START WITH MAXIMUM 0.5 KG POUDER
 

Saul

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NOT REALY

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
-------------------------------------------------- ------------------------------
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 slowly add 1kg of BMK salt. then add 1 liter of sulfonic acid. now connect the reflux and heat the contents of the flask to max temperature. plus minus 130°c. use a powerful mixer
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.
 

Bartholomeus

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Thanks for update Saul
What was the yield from this 1kg reaction?
And what is the purity of your sulfonic acid?
 

Saul

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main ingredient sulfonic acid strength is 75% CAS 7664-38-2
 

pantona123

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@Saul
Thanks for sharing your knowledge, I have a question is the oil you got clear or yellow?
Best regards
 

pantona123

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Thank you very much,
Okay and now to get it clear you have to wash/filter it with dcm right?
Thanks
 
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