Syntese af 1-phenyl-2-propanon (P2P) fra diethyl(phenylacetyl)malonat
- Thread starter G.Patton
- Start date
Mener du simpel destillation i stedet for vakuumdestillation? Det kan du godt, 216 grader C er kogepunktet under normale forhold.
Lad være med at falde for kulten omkring den hellige refluks. Refluks har ingen værdi i sig selv, bortset fra den illusion om, at der sker noget, som det skaber.
Med H2SO4 og oxalsyre (bedst), men fosforsyre og næsten enhver organisk syre som eddikesyre, myresyre eller citronsyre får man næsten kvantitative udbytter, hvis man opvarmer blandingen langsomt over to timer til IKKE MERE end 95 °C, holder den der i 30 minutter og derefter lader den køle ned. Tilsæt en lille mængde andet opløsningsmiddel end DCM (toluen, xylen, ether), da organisk syre kan falde ud, og det anbefales derfor at opsamle fra toppen. Petrol Ether 40/60 kan bruges, og der er ikke brug for meget, men du får TRE lag i sidste ende: Det øverste lag er Pet-Ether med P2P opløst. Mellemste lag er P2P med Pet-Ether opløst*. Og nedenunder er syreblandingen (som i øvrigt kan genbruges uden problemer).
*Det lyder sjovt, men det er sådan, det er: Både Pet-Ether og P2P opløser noget af det andet, men de er ikke frit blandbare. Og så får du de tre lag, som drev mig til vanvid allerede for længe siden. Indtil jeg fandt ud af dette.......
200 g oxalsyre dihydrat
300 ml vand
100 ml H2SO4 37% (batterisyre)
ikke al oxalsyre opløses - ikke noget problem
Med dette kan man behandle mindst 200 ml 20230 rød olie
Der er brug for virkelig kraftig omrøring hele tiden.
Vand/syre-blandingen kan genbruges.
Ikke over 95 °C giver lysegul P2P direkte uden damp eller anden destillation.
Når du bruger en sep-tragt, er det bedst at adskille, så længe det stadig er varmt, og oxalsyren ikke falder ud, eller du lægger det i et bægerglas i fryseren med bunden af bægerglasset i berøring med kulden, så det begynder at krystallisere derfra. Hvis du gør det, behøver du slet ikke noget opløsningsmiddel, for syren og vandet, der krystalliserer fra bunden, vil drive P2P op til toppen, og du kan bare hælde det ud efter to eller tre timer, og der vil IKKE være noget P2P tilbage.
Jeg har lavet en masse arbejde på den her, lol
Med H2SO4 og oxalsyre (bedst), men fosforsyre og næsten enhver organisk syre som eddikesyre, myresyre eller citronsyre får man næsten kvantitative udbytter, hvis man opvarmer blandingen langsomt over to timer til IKKE MERE end 95 °C, holder den der i 30 minutter og derefter lader den køle ned. Tilsæt en lille mængde andet opløsningsmiddel end DCM (toluen, xylen, ether), da organisk syre kan falde ud, og det anbefales derfor at opsamle fra toppen. Petrol Ether 40/60 kan bruges, og der er ikke brug for meget, men du får TRE lag i sidste ende: Det øverste lag er Pet-Ether med P2P opløst. Mellemste lag er P2P med Pet-Ether opløst*. Og nedenunder er syreblandingen (som i øvrigt kan genbruges uden problemer).
*Det lyder sjovt, men det er sådan, det er: Både Pet-Ether og P2P opløser noget af det andet, men de er ikke frit blandbare. Og så får du de tre lag, som drev mig til vanvid allerede for længe siden. Indtil jeg fandt ud af dette.......
200 g oxalsyre dihydrat
300 ml vand
100 ml H2SO4 37% (batterisyre)
ikke al oxalsyre opløses - ikke noget problem
Med dette kan man behandle mindst 200 ml 20230 rød olie
Der er brug for virkelig kraftig omrøring hele tiden.
Vand/syre-blandingen kan genbruges.
Ikke over 95 °C giver lysegul P2P direkte uden damp eller anden destillation.
Når du bruger en sep-tragt, er det bedst at adskille, så længe det stadig er varmt, og oxalsyren ikke falder ud, eller du lægger det i et bægerglas i fryseren med bunden af bægerglasset i berøring med kulden, så det begynder at krystallisere derfra. Hvis du gør det, behøver du slet ikke noget opløsningsmiddel, for syren og vandet, der krystalliserer fra bunden, vil drive P2P op til toppen, og du kan bare hælde det ud efter to eller tre timer, og der vil IKKE være noget P2P tilbage.
Jeg har lavet en masse arbejde på den her, lol
↑View previous replies…
- By w2x3f5
Angiv venligst udbyttet af stoffet p2p.
Har du rød olie? Mærkeligt nok havde jeg gul olie under det samme nummer.
Har du rød olie? Mærkeligt nok havde jeg gul olie under det samme nummer.
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.