Fenilacetono (P2P) sintezė iš benzaldehido su butanonu

William D.

Expert
Joined
Jul 19, 2021
Messages
1,060
Reaction score
1,338
Points
113
Ne, tai bus kitoks kelias. Acetoksis tik su peracto rūgštimi.
 

mewnmewamine

Don't buy from me
New Member
Language
🇺🇸
Joined
May 31, 2025
Messages
115
Reaction score
41
Points
28
No it is also acetoxy
 

Attachments

  • sTiyjLmEfN.png
    sTiyjLmEfN.png
    190.1 KB · Views: 28

Fenster

Don't buy from me
New Member
Joined
Oct 26, 2022
Messages
92
Reaction score
34
Points
8
Ketinu išbandyti šią sintezę su dichlormetanu (DCM). Nematau, kad tai būtų problema, tik kad jis bus sunkesnis už vandenį. Ar yra priežasčių nenaudoti lengvai prieinamo DCM ir sintetinti chloroformą?
 

mewnmewamine

Don't buy from me
New Member
Language
🇺🇸
Joined
May 31, 2025
Messages
115
Reaction score
41
Points
28
Bisulfite adduct is easier and produces a higher purity
 

Fenster

Don't buy from me
New Member
Joined
Oct 26, 2022
Messages
92
Reaction score
34
Points
8
Aldolio kondensacija.

Šios instrukcijos pateiktos skyriuje Organinės reakcijos



Atrodo, kad šis rašinys labiau atitinka tai, ką matau. Ar kas nors iš tikrųjų bandė ekstrahuoti tirpikliu iš organinio sluoksnio. Naudojant chloroformą nepavyks, nes jis maišosi su organiniu sluoksniu. Jei aš kažko nepraleidžiu, šį aprašymą reikia išbandyti ir pakeisti.

Ar kas nors anksčiau bandė šį sintezatorių.
 

TheNut22

Don't buy from me
Resident
Language
🇬🇧
Joined
Feb 12, 2024
Messages
186
Reaction score
92
Points
28
GERAI. Tiesiog kaitinkite benzhidą ir MEK su druskos rūgštimi apie 3-5 valandas. Temperatūra: 90-110 C.
Tiesiog padėkokite man. :)
 
View previous replies…

handle

Don't buy from me
Resident
Language
🇺🇸
Joined
Apr 16, 2023
Messages
207
Reaction score
125
Points
43
 

lalalander

Don't buy from me
Resident
Language
🇺🇸
Joined
Jun 17, 2023
Messages
107
Reaction score
43
Points
28
Visi sako, kad šis metodas turi trūkumų. Ar kas nors, naudodamasis šiuo metodu, kada nors iš tikrųjų gavo didelį derlių?
 

Ortist

Don't buy from me
Resident
Joined
Apr 29, 2023
Messages
89
Solutions
1
Reaction score
55
Points
18
Šį metodą taikiau daugybę kartų. Šiek tiek pakeistas. Geriausius rezultatus gavau 30 ml P2P iš 100 ml benzaldehido. Taip pat pažįstu keletą žmonių, kurie daug tyrinėjo šią reakciją; jų geriausi rezultatai buvo apie 35 ml P2P.

Darbo metodas:

1. Metilfenil-butenonas paruošiamas taip: 500 ml benzaldehido sumaišoma su 1000 ml MEK. Mišinys atšaldomas ledu pripildytame kibire iki maždaug +5 laipsnių.
2. Į jį įpilama 35-37 % vandeninio HCL (reikia įpilti 100 g gryno HCL, kuris atitinka maždaug 286 ml 37 % HCL).
3. Sumaišoma ir laikoma kibire su ledu per naktį, kad ledas ištirptų.
4. Palaukite dar 24 val.
5. Supilkite į skiriamąjį piltuvą, apatinį sluoksnį išmeskite.
6. Tamsiai rudai raudoną mišinį nuplaukite 500 ml vandens, vandenį išmeskite.
7. Distiliuokite viską, kas verda žemesnėje nei 150 laipsnių temperatūroje esant atmosferiniam slėgiui, ir išmeskite
8. Likusią dalį distiliuokite vakuume, kad gautumėte geltoną aliejų

Šis aliejus stovėdamas patamsės per savaitę.


Bayer-Villiger:
1. 100 ml pirmiau paruošto aliejaus įpilkite į 300 ml ledinės acto rūgšties ir 100 ml 50 % vandenilio peroksido mišinio.
2. Kaitinkite ir maišykite 55 laipsnių temperatūroje.
3. Kai reakcija prasidės, temperatūra pakils virš 55..60 (apie 1..2 val.): tai yra rodiklis, rodantis, kad reikia išjungti kaitinimą. Jei temperatūra pakyla iki 70, tuomet šiek tiek atvėsinkite kolbą po tekančiu vandeniu.
4. Maišykite, kol temperatūra nukris iki 50-55 laipsnių, tada vėl įjunkite kaitinimą
5. Maišykite ir kaitinkite 6 valandas
7. Mišinį supilkite į 1 l vandens, ekstrahuokite 3 kartus su 100+100+100 ml DCM
8. Išdistiliuokite DCM


Saponifikacija:
1. Į kolbą maišant supilkite Bayer-Villigerio produktą, gautą ankstesniame etape. Lėtai įpilkite
NaOH tirpalą (30 g NaOH, 250 ml vandens, 250 ml etanolio). Lėtai, t. y. po lašelį, maždaug po 3..5 lašus per sekundę. Mišinys tampa rausvai oranžinis

2. Baigiant pilti pH turi būti didesnis nei 12
3. Į mišinį įpilkite acto rūgšties (bet kokiu procentu) iki neutralaus pH. Mišinys taps geltonas
4. Supilkite jį į 1 l vandens ir ekstrahuokite 3 kartus su 100+100+100 ml DCM
5. DCM ir etanolio pėdsakus distiliuokite esant atmosferos slėgiui
6. P2P distiliuokite vakuume.
7. Kolboje liks daug deguto
 
View previous replies…

RainbowChemical

Don't buy from me
New Member
Language
🇺🇸
Joined
Jul 29, 2025
Messages
1
Reaction score
1
Points
1
I just wanted to point out that there are new studies done about this. The more MEK that is used the less byproducts that are formed. In the study I read they used a ratio of 1 to 6 (1 benzaldehyde to 6 MEK) but when they increased this amount to 8 times and 10 times all byproducts disappeared
 

TheNut22

Don't buy from me
Resident
Language
🇬🇧
Joined
Feb 12, 2024
Messages
186
Reaction score
92
Points
28
10 g benzaldehido + 24 g MEK + 28 g vandenilio rūgšties (~20%) = 28 g kristalų, išdžiovintų pirekso lėkštelėje = 13 g kristalų.
Paprasčiausiai. Baigę kaitinti, išskobkite rudą organinį sluoksnį. Nuplaukite 40 ml vandens. Vėl ekstrahuokite. Įpilkite 20 ml:s 10 % KOH tirpalo. Atsikratykite vandens. Patikrinkite pH. Jei jis per rūgštus arba per šarminis, nustatykite 7. Vėl išpilkite vandenį. Įdėkite į šaldiklį, nes užšaldžius galima išpilti riebų šūdą ir gauti beveik baltus kristalus. Įdėkite kristalus į pirekso indą ar ką nors panašaus ir išdžiovinkite. Jis gali suskystėti, bet ne problema. Tiesiog kaitinkite, šaldykite, kaitinkite, šaldykite, džiovinkite tuos kristalus, bet jie negali būti traškūs sausi. Nežinau kodėl. Gal jie tiesiog tokie yra.
 
Last edited:
View previous replies…

chema12

Don't buy from me
New Member
Language
🇪🇸
Joined
Jul 3, 2025
Messages
0
Reaction score
0
Points
1
Deleted
View previous replies…

Kodey

Don't buy from me
Resident
Language
🇹🇷
Joined
Dec 5, 2024
Messages
11
Reaction score
1
Points
3
Can 3-methyl-4-phenyl-3-buten-2-one be distilled without vacuum?
 

waltjr5858

Don't buy from me
Resident
Language
🇺🇸
Joined
Apr 5, 2024
Messages
89
Reaction score
19
Points
8
Lol it turned to some bad stuff without vac... I went on to the next step the next time with some minor cleaning and no distillation....I didn't clean up till the end with steam distillation... works fine... yield still plenty good enough. I hate the way that stuff vac distilled......
 

Kodey

Don't buy from me
Resident
Language
🇹🇷
Joined
Dec 5, 2024
Messages
11
Reaction score
1
Points
3
Yk vacuum distillation is some kind of demon creation thing
 

waltjr5858

Don't buy from me
Resident
Language
🇺🇸
Joined
Apr 5, 2024
Messages
89
Reaction score
19
Points
8
Yup so it wasn't just me... thought I screwed something up but it's pretty easy at that point HA. I've now gotten through the entire thing and just doing a steam distillation at the end and it turns out perfectly every time. Although it took some tries to get there.
 

chem lover

Don't buy from me
Member
Language
🇺🇸
Joined
May 17, 2025
Messages
12
Reaction score
0
Points
1
Can i use 35% H2O2 instead of 50%?
 

Chemtrail

Don't buy from me
Resident
Language
🇺🇸
Joined
May 10, 2025
Messages
424
Reaction score
103
Points
28
Synthesis of benzaldehyde
 

Attachments

  • 80jsDJRO4v.png
    80jsDJRO4v.png
    443.2 KB · Views: 31
  • ykwpsQHVgP.png
    ykwpsQHVgP.png
    469 KB · Views: 32

mewnmewamine

Don't buy from me
New Member
Language
🇺🇸
Joined
May 31, 2025
Messages
115
Reaction score
41
Points
28
Too much GAA use maybe 1.6lish

Hydrolysis is too long in my exp
1.25eq base and 2hrs worked best for me

you didnt get 50% peroxide and attempt this 💀 will d scale up no testing time again

Purification via methylphenylbutanones bisulfite adduct is so much superior (same with p2p) both for not having to make chloroforms sake and end purity

huge excess of mek? Intentional? also amino acids r a better cat than hcl for the aldol and id use perborate for the villiger as thats higher yielding in my exp than H2O2. Percarbonate is less good getting maybe 35% but much easier and not watched at all
 

lalalander

Don't buy from me
Resident
Language
🇺🇸
Joined
Jun 17, 2023
Messages
107
Reaction score
43
Points
28
I'm considering purifying P2P using bisulfite, but I've read many times that the recovery is low. What is the yield after re-liberating it from the bisulfite adduct?
 
View previous replies…

mewnmewamine

Don't buy from me
New Member
Language
🇺🇸
Joined
May 31, 2025
Messages
115
Reaction score
41
Points
28
80s and 90s just try not to have much water in solution as bisulfite adducts are annoyingly slightly soluble in them :3
 

mewnmewamine

Don't buy from me
New Member
Language
🇺🇸
Joined
May 31, 2025
Messages
115
Reaction score
41
Points
28
Oh wait! U can salt it out too cos its only a tiny bit soluble
 

lalalander

Don't buy from me
Resident
Language
🇺🇸
Joined
Jun 17, 2023
Messages
107
Reaction score
43
Points
28
Does MPB form a bisulfite adduct? No matter how many times I tried, I wasn’t successful. I tried with water, and with a methanol-water mixture. It just doesn’t work.
 

lalalander

Don't buy from me
Resident
Language
🇺🇸
Joined
Jun 17, 2023
Messages
107
Reaction score
43
Points
28
The suspected P2P adduct was left to dry on the filter. Right now, its texture is indistinguishable from that of a mica-based eyeshadow — it looks exactly like it. Like phenylacetic acid. Is this normal?
 

nokospp

Don't buy from me
Member
Language
🇺🇸
Joined
May 30, 2025
Messages
8
Reaction score
0
Points
3
is this route can be scaled down ?
 

mewnmewamine

Don't buy from me
New Member
Language
🇺🇸
Joined
May 31, 2025
Messages
115
Reaction score
41
Points
28
Things essentially always work scaled down its scaling up where things go wrong you should be good :3
 
Top