Ne, to bo drugačna pot. Acetoksi samo s perocetno kislino.
Sinteza fenilacetona (P2P) iz benzaldehida z butanonom
- Thread starter William D.
- Start date
Poskusil bom to sintezo z diklorometanom (DCM). Ne vidim, da bi to predstavljalo težavo, le da bo težji od vode. Ali je kakršen koli razlog, da ne bi uporabili lahko dostopnega DCM in kloroforma za sintezo?
Aldolova kondenzacija.
Navodila za to so v poglavju Organske reakcije
Zdi se, da se ta zapis bolj ujema s tem, kar vidim. Ali je kdo dejansko poskušal ekstrahirati s topilom iz organske plasti. Uporaba kloroforma ne bo delovala, ker se meša z organsko plastjo. Če nisem česa spregledal, je treba zapis preizkusiti in spremeniti.
Ali je kdo že poskusil ta sintetizator.
Navodila za to so v poglavju Organske reakcije
Zdi se, da se ta zapis bolj ujema s tem, kar vidim. Ali je kdo dejansko poskušal ekstrahirati s topilom iz organske plasti. Uporaba kloroforma ne bo delovala, ker se meša z organsko plastjo. Če nisem česa spregledal, je treba zapis preizkusiti in spremeniti.
Ali je kdo že poskusil ta sintetizator.
- By TheNut22
V REDU. Samo segrevajte benzhid in MEK s klorovodikovo kislino približno 3-5 ur. Temperatura: 90-110 C.
Samo zahvalite se mi.
Samo zahvalite se mi.
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letmegooglethat.com
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Translate To English!
For those who think it's easier to annoy you than to Google 'Translate to english!' themselves.
10 g benzaldehida + 24 g MEK + 28 g hidrokisline (~20 %) = 28 g kristalov, posušenih v posodi iz stekla pyrex = 13 g kristalov.
Naj bo preprosto. Ko končate s segrevanjem, izločite rjavo organsko plast. Izperite s 40 ml vode. Ponovno ekstrahirajte. Dajte 20 ml:s 10-odstotne raztopine KOH. Znebite se vode. Preverite pH. Če je preveč kisel ali preveč bazičen, ga povečajte na 7. Ponovno se znebite vode. Dajte v zamrzovalnik, ker lahko potem, ko je zamrznjeno, odcedite mastno sranje in dobite skoraj bele kristale. Kristale dajte v posodo iz pireksa ali kaj podobnega in jih posušite. Lahko se utekočinijo, vendar brez težav. Samo segrevajte, zamrzujte, segrevajte, zamrzujte, posušite te kristale, vendar ne morejo biti hrustljavo suhi. Ne vem, zakaj. Morda so pač takšni.
Naj bo preprosto. Ko končate s segrevanjem, izločite rjavo organsko plast. Izperite s 40 ml vode. Ponovno ekstrahirajte. Dajte 20 ml:s 10-odstotne raztopine KOH. Znebite se vode. Preverite pH. Če je preveč kisel ali preveč bazičen, ga povečajte na 7. Ponovno se znebite vode. Dajte v zamrzovalnik, ker lahko potem, ko je zamrznjeno, odcedite mastno sranje in dobite skoraj bele kristale. Kristale dajte v posodo iz pireksa ali kaj podobnega in jih posušite. Lahko se utekočinijo, vendar brez težav. Samo segrevajte, zamrzujte, segrevajte, zamrzujte, posušite te kristale, vendar ne morejo biti hrustljavo suhi. Ne vem, zakaj. Morda so pač takšni.
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- By TheNut22
Vendar je tu ena nenavadna stvar. Ko sploh ne merim ravni pH in te bele kristale samo položim v merilno bučko v zamrzovalnik, dobim dvojno količino čistih belih kristalov. Danes sem pripravil skoraj enako količino reagentov in na enak način, ALE ko sem titriral pH-raven na 7, sem dobil le polovico kristalov. Mislim, da je nekaj na tem. Sedaj zvečer sem dal teh 20 ml kristalov v zamrzovalnik in so oranžni! polovica je videti, kot da bi lahko dobili samo olje, vendar sem preveril, da je prišlo do neke reakcije med oranžno raztopino in zgornjo plastjo belih kristalov, ki so se pojavili v približno 10 minutah. Prišel sem do zaključka, da ko narediš aldol s kislino in dobiš bazične kristale ter sploh ne titriraš pH-ravni, dobiš dvojno ali trojno količino metilfenilbutenona, in ko je to čez noč v zamrzovalniku, v zgornjo plast spustiš olje in to je to. Zato od zdaj naprej ne priporočam titracije pH-ravni.
P.S Oprostite, danes sem naredil nekaj metkatinona in sem zelo utrujen, zato se opravičujem za nejasno besedilo.
Zdaj grem spat.
P.S Oprostite, danes sem naredil nekaj metkatinona in sem zelo utrujen, zato se opravičujem za nejasno besedilo.
Zdaj grem spat.
Can 3-methyl-4-phenyl-3-buten-2-one be distilled without vacuum?
- By waltjr5858
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......
- By waltjr5858
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.
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
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 againPurification 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
- By lalalander
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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- By mewnmewamine
80s and 90s just try not to have much water in solution as bisulfite adducts are annoyingly slightly soluble in them :3
- By lalalander
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.
- By lalalander
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?
is this route can be scaled down ?
- By mewnmewamine
Things essentially always work scaled down its scaling up where things go wrong you should be good :3