Fenilacetona (P2P) sintēze no benzaldehīda ar butanonu

William D.

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Nē, tas būs cits ceļš. Acetoksi tikai ar perietiķskābi.
 

mewnmewamine

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No it is also acetoxy
 

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Fenster

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Es grasos izmēģināt šo sintēzi ar dihlormetānu (DCM). Es neredzu, ka tas būtu problēma, tikai tas, ka tas būs smagāks par ūdeni. Vai ir kādi iemesli, lai neizmantotu viegli pieejamo DCM un nesintezētu hloroformu?
 

mewnmewamine

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Bisulfite adduct is easier and produces a higher purity
 

Fenster

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Aldola kondensācija.

Norādījumi par to ir iekļauti sadaļā Organiskās reakcijas



Šķiet, ka šis uzraksts vairāk atbilst tam, ko es redzu. Vai kāds patiešām ir mēģinājis ekstrahēt ar šķīdinātāju no organiskā slāņa. Hloroforma izmantošana nedarbosies, jo tas ir sajaucams ar organisko slāni. Ja vien es kaut ko nepalaidu garām, šis apraksts ir jāpārbauda un jāmaina.

Vai kāds jau ir mēģinājis šo sintētisko vielu.
 

TheNut22

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LABI. Vienkārši karsē benzhīdu un MEK ar sālsskābi apmēram 3-5 stundas. Temperatūra: 90-110 C.
Tikai paldies man. :)
 
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chema12

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Hola amigó...podría ayudarme con la cintesis..tengo ese producto..
Me gustaría q me ayudara a cintetisar mi p2p apartir de benzaldehido
 

handle

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TheNut22

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10 g benzaldehīda + 24 g MEK + 28 g hidr.skābes (~20%) = 28 g kristālu, izžāvēti pyrex traukā = 13 g kristālu.
Vienkārši. Kad esat pabeidzis karsēšanu, ekstrahējiet brūno organisko slāni. Noskalojiet ar 40 ml ūdens. Vēlreiz ekstrahē. Ielej 20 ml:s 10 % KOH šķīduma. Atbrīvojieties no ūdens. Pārbaudiet pH. Ja tas ir pārāk skābs vai pārāk bāzisks, palieliniet to līdz 7. Atkal atbrīvojieties no ūdens. Ielieciet to saldētavā, jo tad, kad tas ir sasaldēts, var izliet eļļoto sūdus un iegūt gandrīz baltus kristālus. Ievietojiet kristālus pyrex traukā vai kādā citā traukā un žāvējiet. Tas var sašķidrināties, bet nav problēmu. Vienkārši karsē, sasaldē, karsē, sasaldē, tu žāvē tos kristālus, bet tie nevar būt kraukšķīgi sausi. Nezinu, kāpēc. Varbūt tie vienkārši tādi ir.
 
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TheNut22

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Taču ir viena dīvaina lieta. Ja es nemaz nemērīšu pH līmeni un vienkārši ielieku šos baltos kristālus mērkolbā saldētavā, es iegūstu dubultu tīru baltu kristālu daudzumu. Šodien es pagatavoju gandrīz tādu pašu reaģentu daudzumu un tādā pašā veidā, BET es titrēju pH līmeni līdz 7, un es dabūju tikai pusi kristālu. Es domāju, ka kaut kas ar to ir saistīts. Tagad vakarā es tikko ieliku tos 20 ml kristālu saldētavā, un tie ir oranži! puse no tiem izskatās, ka varētu iegūt tikai eļļu, bet es tikko pārbaudīju, ka ir kāda reakcija starp oranžo šķīdumu un augšējā slāņa baltajiem kristāliem, kas parādījās apmēram 10 minūšu laikā. Es nonācu pie secinājuma, ka, veicot aldola reakciju ar skābi un iegūstot bāziskus kristālus un nemaz netitrējot pH līmeni, iegūst divkāršu vai trīskāršu metilfenilbutenona daudzumu, un, kad tas uz nakti atrodas saldētavā, augšējā slānī izlej eļļu, un viss. Tāpēc turpmāk es neiesaku titrēt pH līmeni.

P.S Atvainojos, šodien pagatavoju metkatinonu un esmu ļoti noguris, tāpēc atvainojos par neskaidro tekstu.
Tagad eju gulēt.
 
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chema12

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Me podrías ayudar con la cintesis..xfa
 

Kodey

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Can 3-methyl-4-phenyl-3-buten-2-one be distilled without vacuum?
 

waltjr5858

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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

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Yk vacuum distillation is some kind of demon creation thing
 

waltjr5858

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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

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Can i use 35% H2O2 instead of 50%?
 

Chemtrail

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Synthesis of benzaldehyde
 

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mewnmewamine

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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
 

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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?
 
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mewnmewamine

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80s and 90s just try not to have much water in solution as bisulfite adducts are annoyingly slightly soluble in them :3
 

mewnmewamine

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Oh wait! U can salt it out too cos its only a tiny bit soluble
 

lalalander

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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

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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

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is this route can be scaled down ?
 

mewnmewamine

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Things essentially always work scaled down its scaling up where things go wrong you should be good :3
 
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