Sinteza 1-fenil-2-propanona (P2P) iz dietil(fenilacetil)malonata
- Thread starter G.Patton
- Start date
Ali imate v mislih preprosto destilacijo namesto vakuumske? Lahko, 216 stopinj C je vrelišče pri normalnih pogojih.
Fantje, ne nasedajte kultu svetega refluksa. Refluksiranje samo po sebi nima nobene vrednosti, razen iluzije, da se nekaj dogaja, ki jo ustvarja.
Z H2SO4 in oksalno kislino (najbolje), pa tudi s fosforno kislino in katero koli organsko kislino, kot so ocetna, mravljinčna ali citronska, lahko dosežemo skoraj kvantitativne rezultate, če zmes počasi segrevamo dve uri na 95 °C, jo zadržimo 30 minut in jo nato ohladimo. Dodajte majhno količino topila, ki ni DCM (toluen, ksilen, eter), saj lahko organska kislina izpade, zato se priporoča zbiranje z vrha. Uporabimo lahko bencinski eter 40/60 in ne potrebujemo veliko, vendar na koncu dobimo TRI plasti: Zgornja plast je petrol eter z raztopljenim P2P. Srednja plast je P2P z raztopljenim pet-etrom*. Spodaj pa je mešanica kisline (ki se lahko brez težav ponovno uporabi).
*Zveni smešno, vendar je tako: Pet-eter in P2P raztopita nekaj drugega, vendar se ne mešata prosto. Tako dobimo tri plasti, ki so me že pred časom spravile ob živce. Dokler nisem ugotovil tega.......
200 g oksalne kisline dihidrata
300 ml vode
100 ml H2SO4 37 % (baterijska kislina)
vsa oksalna kislina se ne bo raztopila - ni problema
S tem lahko predelamo najmanj 200 ml rdečega olja 20230
Ves čas je potrebno zelo močno mešanje.
Mešanico vode in kisline lahko ponovno uporabite.
Ne več kot 95 °C daje svetlo rumeno P2P neposredno, brez pare ali druge destilacije.
Kadar uporabljate ločilni lonček, najbolje ločite, dokler je še vroče in oksalna kislina ne izpade. ali pa ga dajte v čašo v zamrzovalnik, pri čemer se dno čaše dotika hladnega, tako da začne kristalizirati od tam. Če to storite, ne potrebujete nobenega topila, kislina in voda, ki kristalizirata z dna, potisneta P2P na vrh in po dveh ali treh urah ga lahko preprosto odlijete, pri čemer P2P ne bo ostal nazaj.
Pri tem sem se zelo potrudil, lol
Z H2SO4 in oksalno kislino (najbolje), pa tudi s fosforno kislino in katero koli organsko kislino, kot so ocetna, mravljinčna ali citronska, lahko dosežemo skoraj kvantitativne rezultate, če zmes počasi segrevamo dve uri na 95 °C, jo zadržimo 30 minut in jo nato ohladimo. Dodajte majhno količino topila, ki ni DCM (toluen, ksilen, eter), saj lahko organska kislina izpade, zato se priporoča zbiranje z vrha. Uporabimo lahko bencinski eter 40/60 in ne potrebujemo veliko, vendar na koncu dobimo TRI plasti: Zgornja plast je petrol eter z raztopljenim P2P. Srednja plast je P2P z raztopljenim pet-etrom*. Spodaj pa je mešanica kisline (ki se lahko brez težav ponovno uporabi).
*Zveni smešno, vendar je tako: Pet-eter in P2P raztopita nekaj drugega, vendar se ne mešata prosto. Tako dobimo tri plasti, ki so me že pred časom spravile ob živce. Dokler nisem ugotovil tega.......
200 g oksalne kisline dihidrata
300 ml vode
100 ml H2SO4 37 % (baterijska kislina)
vsa oksalna kislina se ne bo raztopila - ni problema
S tem lahko predelamo najmanj 200 ml rdečega olja 20230
Ves čas je potrebno zelo močno mešanje.
Mešanico vode in kisline lahko ponovno uporabite.
Ne več kot 95 °C daje svetlo rumeno P2P neposredno, brez pare ali druge destilacije.
Kadar uporabljate ločilni lonček, najbolje ločite, dokler je še vroče in oksalna kislina ne izpade. ali pa ga dajte v čašo v zamrzovalnik, pri čemer se dno čaše dotika hladnega, tako da začne kristalizirati od tam. Če to storite, ne potrebujete nobenega topila, kislina in voda, ki kristalizirata z dna, potisneta P2P na vrh in po dveh ali treh urah ga lahko preprosto odlijete, pri čemer P2P ne bo ostal nazaj.
Pri tem sem se zelo potrudil, lol
↑View previous replies…
- By w2x3f5
Navedite količino snovi p2p, prosimo.
ali imate rdeče olje? nenavadno je, da sem imel pod isto številko rumeno olje.
ali imate rdeče olje? nenavadno je, da sem imel pod isto številko rumeno olje.
Is there any other way to isolate the phenylacetic acid besides putting it in the refrigerator? Will not separating affect my future work?
- By William D.
You can crystallize this in a cool place and filter after. In another case, you can distill the fractions. For the following steps, you cannot leave PPA.
I would like to know if this synthesis is also working with phosphoric acid ( h3pO4) I appreciate your work and time
And what would be the amount ( phosphoric acid 85%)
Currently performing a test on the substrate with 75% phosphoric acid. No exact amounts used.
Trying with about 1:2 (Precursor to Phosphoric acid), again no exact amounts used but will report back if it works at all.
Trying with about 1:2 (Precursor to Phosphoric acid), again no exact amounts used but will report back if it works at all.
Tests using 75% phosphoric acid 1:2 (substrate to acid). 1 hour and 30 minutes into the reaction. Took a small "sniff test" and I seem to be able to detect the distinct odour of phenyl-2-propanone.
Lots of bubbling in the reaction that started as early as 60 degress celcius.
Again no exact amounts was actually used as the substrate I tried was a sample purchase from a chinese vendor (not on this site). Red liquid just like the photos of the malonate everywhere, the smell was not super pleasant but not horrible. Around 100 euro per kilo (actually less considering shipping was included)
Lots of bubbling in the reaction that started as early as 60 degress celcius.
Again no exact amounts was actually used as the substrate I tried was a sample purchase from a chinese vendor (not on this site). Red liquid just like the photos of the malonate everywhere, the smell was not super pleasant but not horrible. Around 100 euro per kilo (actually less considering shipping was included)
2 hours and 23 minutes into the reaction and I can confirm 100% that 75% phosphoric acid definitely works. However the reaction is still bubbling from CO2 evolution, so the reaction is not done.
The smell of phenyl-2-propanone is now too strong to dispute. The substrate was legit.
Further experimentation needs to be done to determine optimal amount of phosphoric acid.
Previous experience: [P2NP (from benzaldehyde & nitroethane) to phenyl-2-propanone with iron powder and HCL] and [MAPA to phenyl-2-propanone with hydrochloric acid])
If I remember correctly the p2np to phenyl-2-propanone with iron powder and HCL sometimes produced phenyl-2-propanone with an acrid smell. however the smell of the phenyl-2-propanone from the malonate is extremely sweet and that of pure phenyl-2-propanone.
Will store the resulting phenyl-2-propanone as a powder by reacting it with metabisulfite.
edit: Also beware of alibaba sellers of BMK precursors, one of them was not legit. (check the bot reviews, the fake sellers strictly sell precursors and have fake reviews of GBL and synthetic cannabinoid indole derivatives)
The smell of phenyl-2-propanone is now too strong to dispute. The substrate was legit.
Further experimentation needs to be done to determine optimal amount of phosphoric acid.
Previous experience: [P2NP (from benzaldehyde & nitroethane) to phenyl-2-propanone with iron powder and HCL] and [MAPA to phenyl-2-propanone with hydrochloric acid])
If I remember correctly the p2np to phenyl-2-propanone with iron powder and HCL sometimes produced phenyl-2-propanone with an acrid smell. however the smell of the phenyl-2-propanone from the malonate is extremely sweet and that of pure phenyl-2-propanone.
Will store the resulting phenyl-2-propanone as a powder by reacting it with metabisulfite.
edit: Also beware of alibaba sellers of BMK precursors, one of them was not legit. (check the bot reviews, the fake sellers strictly sell precursors and have fake reviews of GBL and synthetic cannabinoid indole derivatives)
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Appreciate your work hope we can get a detailed syntheses of phosphoric acid. I have 85% of phosphoric acid and hope to find a way that is working
Take notice: Ignore the 5 hour bullshit, it was not enough for me with 75% phosphoric acid. I ended up with way too much oil than theoretically possible. i.e. it was a mixture of the precursor and product, the precursor had not fully reacted. (I also detected the precursor smell when working up the reaction). This is a big problem according to me as they are annoying to separate from eachother. Therefor it is important, imo, to run the reaction to completion, I'd rather have bi-products or some slight polymerisation from running the reaction longer than unreacted precursor.
Better to end the reaction when it no longer is bubbling or bubbling very little.
Also don't wait for a detailed guide. Just try it yourself using small amounts.
Either use a 1:1 or 1:2 ratio of precursor to phosphoric acid. This is not that complex.
Better to end the reaction when it no longer is bubbling or bubbling very little.
Also don't wait for a detailed guide. Just try it yourself using small amounts.
Either use a 1:1 or 1:2 ratio of precursor to phosphoric acid. This is not that complex.