1-fenil-2-propanona (P2P) sintēze no dietil(fenilacetil)malonāta
- Thread starter G.Patton
- Start date
Vai jūs domājat vienkāršu destilāciju, nevis vakuumdestilāciju? Varat, 216 grādi C ir viršanas temperatūra normālos apstākļos.
Puiši, neaizraujieties ar svētā refluksa kultu. Refluksam pašam par sevi nav nekādas vērtības, izņemot ilūziju, ka kaut kas notiek, ko tas rada.
Izmantojot H2SO4 un skābeņskābi (vislabāk), bet fosforskābi un jebkuru organisko skābi, piemēram, etiķskābi, skudrskābi vai citronskābi, var iegūt gandrīz kvantitatīvu iznākumu, ja maisījumu divas stundas lēnām uzkarsē līdz 95 °C, tur 30 minūtes un tad ļauj atdzist. Pievieno nelielu daudzumu šķīdinātāja, kas nav DCM (toluols, ksilols, ēteris), jo organiskā skābe var izkrist, tāpēc ieteicams to savākt no augšas. Var izmantot benzīna ēteri 40/60, un nav vajadzīgs daudz, bet beigās iegūst trīs slāņus: Augšējais slānis ir petēteris ar izšķīdušu P2P. Vidējais slānis ir P2P ar izšķīdušu petēteri*. Zemāk ir skābes maisījums (ko var izmantot atkārtoti bez problēmām).
* Izklausās smieklīgi, bet tā tas ir: Gan petēteris, gan P2P izšķīdina daļu no otra, bet tie nav brīvi sajaucami. Un tā rodas trīs slāņi, kas mani jau sen atpakaļ izdzina no prāta. Līdz es to sapratu.......
200 g Skābeņskābes dihidrāta
300 ml ūdens
100 ml H2SO4 37% (akumulatora skābe)
ne visa skābeņskābe izšķīst - nav problēmu.
Ar to var apstrādāt vismaz 200 ml 20230 sarkanās eļļas.
Visu laiku ir vajadzīga ļoti spēcīga maisīšana.
Ūdens/skābes maisījumu var izmantot atkārtoti.
Nepārsniedzot 95 °C temperatūru, tiek iegūts gaiši dzeltens P2P tieši bez tvaika vai citas destilācijas.
Ja izmantojat atdalīšanas piltuvi, vislabāk atdalīt, kamēr tā vēl ir karsta un skābeņskābe neizkrīt. vai arī ielieciet to mērglāzē saldētavā, mērglāzes dibenam pieskaroties aukstumam, lai tā no turienes sāktu kristalizēties. Šādā gadījumā šķīdinātājs nav vajadzīgs, jo skābe un ūdens, kas kristalizējas no apakšas, izspiež P2P uz augšu, un pēc divām vai trim stundām to var vienkārši izliet, un P2P nepaliek atpakaļ.
Es pie tā daudz strādāju, lol
Izmantojot H2SO4 un skābeņskābi (vislabāk), bet fosforskābi un jebkuru organisko skābi, piemēram, etiķskābi, skudrskābi vai citronskābi, var iegūt gandrīz kvantitatīvu iznākumu, ja maisījumu divas stundas lēnām uzkarsē līdz 95 °C, tur 30 minūtes un tad ļauj atdzist. Pievieno nelielu daudzumu šķīdinātāja, kas nav DCM (toluols, ksilols, ēteris), jo organiskā skābe var izkrist, tāpēc ieteicams to savākt no augšas. Var izmantot benzīna ēteri 40/60, un nav vajadzīgs daudz, bet beigās iegūst trīs slāņus: Augšējais slānis ir petēteris ar izšķīdušu P2P. Vidējais slānis ir P2P ar izšķīdušu petēteri*. Zemāk ir skābes maisījums (ko var izmantot atkārtoti bez problēmām).
* Izklausās smieklīgi, bet tā tas ir: Gan petēteris, gan P2P izšķīdina daļu no otra, bet tie nav brīvi sajaucami. Un tā rodas trīs slāņi, kas mani jau sen atpakaļ izdzina no prāta. Līdz es to sapratu.......
200 g Skābeņskābes dihidrāta
300 ml ūdens
100 ml H2SO4 37% (akumulatora skābe)
ne visa skābeņskābe izšķīst - nav problēmu.
Ar to var apstrādāt vismaz 200 ml 20230 sarkanās eļļas.
Visu laiku ir vajadzīga ļoti spēcīga maisīšana.
Ūdens/skābes maisījumu var izmantot atkārtoti.
Nepārsniedzot 95 °C temperatūru, tiek iegūts gaiši dzeltens P2P tieši bez tvaika vai citas destilācijas.
Ja izmantojat atdalīšanas piltuvi, vislabāk atdalīt, kamēr tā vēl ir karsta un skābeņskābe neizkrīt. vai arī ielieciet to mērglāzē saldētavā, mērglāzes dibenam pieskaroties aukstumam, lai tā no turienes sāktu kristalizēties. Šādā gadījumā šķīdinātājs nav vajadzīgs, jo skābe un ūdens, kas kristalizējas no apakšas, izspiež P2P uz augšu, un pēc divām vai trim stundām to var vienkārši izliet, un P2P nepaliek atpakaļ.
Es pie tā daudz strādāju, lol
↑View previous replies…
- By w2x3f5
Lūdzu, norādiet vielas p2p iznākumu.
Vai jums ir sarkanā eļļa? dīvaini, bet man zem tā paša numura bija dzeltenā eļļa.
Vai jums ir sarkanā eļļa? dīvaini, bet man zem tā paša numura bija dzeltenā eļļa.
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)
Last edited:
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.