1-fenüül-2-propanooni (P2P) süntees dietüül(fenüülatsetüül)malonaadist
- Thread starter G.Patton
- Start date
Kas te mõtlete vaakumdestillatsiooni asemel lihtsat destillatsiooni? Võite, 216 kraadi C on keemistemperatuur normaaltingimustes.
Poisid, ärge langege püha refluksi kultusesse. Refluksimisel ei ole iseenesest mingit väärtust, välja arvatud illusioon millegi toimumisest, mida see tekitab.
H2SO4 ja oksaalhappega (parim), kuid fosforhappega ja peaaegu iga orgaanilise happega, nagu äädikhape või sipelghape või sidrunhape, saab peaaegu kvantitatiivse saagise, kui segu aeglaselt kahe tunni jooksul kuumutada kuni 95 °C-ni, hoida seda seal 30 minutit ja lasta seejärel jahtuda. Lisage väike kogus muud lahustit kui DCM (tolueen, ksüleen, eeter), sest orgaaniline hape võib välja kukkuda, mistõttu on soovitatav koguda ülevalt. Võib kasutada bensiini eetrit 40/60 ja seda ei ole palju vaja, kuid lõpuks saadakse KOLME kihti: Ülemine kiht on petrooleeter, milles on lahustatud P2P. Keskmine kiht on P2P koos Pet-Etheriga lahustatuna*. Ja allpool on happesegu (mida võib btw. probleemideta uuesti kasutada).
*Kõlab naljakalt, aga nii ongi: Nii Pet-Ether kui ka P2P lahustavad teineteist, kuid thex ei ole vabalt segunevad. Ja nii saabki kolm kihti, mis mind juba ammu kõrvuti hulluks ajas. Kuni ma sellest aru sain.......
200 g oksaalhappe dihüdraat
300 ml vett
100 ml H2SO4 37% (akuhape)
kõik oksaalhape ei lahustu - pole probleemi
Sellega saab töödelda vähemalt 200 ml 20230 punast õli
Tõeliselt tugevat segamist on vaja kogu aeg.
Vee ja happe segu võib uuesti kasutada.
Mitte üle 95 °C annab helekollase P2P otse ilma auru või muu destillatsioonita.
Kui kasutad sep-funnelit siis kõige parem eraldada niikaua kui see veel kuum on ja oksaal ei tilgu välja. või paned selle keeduklaasi sügavkülma nii, et keeduklaasi põhi puutub külma, nii hakkab see sealt kristalliseeruma. Kui te seda teete, siis ei ole teil üldse mingit lahustit vaja, altpoolt kristalliseeruv hape ja vesi ajab P2P üles ja te võite selle lihtsalt kahe või kolme tunni pärast välja valada ja EI jää P2P tagasi.
Ma tegin palju tööd sellega, lol
H2SO4 ja oksaalhappega (parim), kuid fosforhappega ja peaaegu iga orgaanilise happega, nagu äädikhape või sipelghape või sidrunhape, saab peaaegu kvantitatiivse saagise, kui segu aeglaselt kahe tunni jooksul kuumutada kuni 95 °C-ni, hoida seda seal 30 minutit ja lasta seejärel jahtuda. Lisage väike kogus muud lahustit kui DCM (tolueen, ksüleen, eeter), sest orgaaniline hape võib välja kukkuda, mistõttu on soovitatav koguda ülevalt. Võib kasutada bensiini eetrit 40/60 ja seda ei ole palju vaja, kuid lõpuks saadakse KOLME kihti: Ülemine kiht on petrooleeter, milles on lahustatud P2P. Keskmine kiht on P2P koos Pet-Etheriga lahustatuna*. Ja allpool on happesegu (mida võib btw. probleemideta uuesti kasutada).
*Kõlab naljakalt, aga nii ongi: Nii Pet-Ether kui ka P2P lahustavad teineteist, kuid thex ei ole vabalt segunevad. Ja nii saabki kolm kihti, mis mind juba ammu kõrvuti hulluks ajas. Kuni ma sellest aru sain.......
200 g oksaalhappe dihüdraat
300 ml vett
100 ml H2SO4 37% (akuhape)
kõik oksaalhape ei lahustu - pole probleemi
Sellega saab töödelda vähemalt 200 ml 20230 punast õli
Tõeliselt tugevat segamist on vaja kogu aeg.
Vee ja happe segu võib uuesti kasutada.
Mitte üle 95 °C annab helekollase P2P otse ilma auru või muu destillatsioonita.
Kui kasutad sep-funnelit siis kõige parem eraldada niikaua kui see veel kuum on ja oksaal ei tilgu välja. või paned selle keeduklaasi sügavkülma nii, et keeduklaasi põhi puutub külma, nii hakkab see sealt kristalliseeruma. Kui te seda teete, siis ei ole teil üldse mingit lahustit vaja, altpoolt kristalliseeruv hape ja vesi ajab P2P üles ja te võite selle lihtsalt kahe või kolme tunni pärast välja valada ja EI jää P2P tagasi.
Ma tegin palju tööd sellega, lol
↑View previous replies…
- By w2x3f5
märkige aine saagis p2p palun.
kas teil on punane õli? kummalisel kombel oli mul sama numbri all kollane õli.
kas teil on punane õli? kummalisel kombel oli mul sama numbri all kollane õli.
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.