Fenüülatsetooni (P2P) süntees bensaldehüüdist koos butanooniga

MadHatter

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Ma arvan, et mind huvitab tegelikult selle reaktsiooni stöhhiomeetria. Teistes bayer-willigeri kirjutistes ma ei leia seda tohutut kogust GAA-d. Kas keegi oskab mind aidata põhjendusega? Olen tõesti lähedal sellele, et seda proovida, kuid GAA kogus on problemaatiline.
 

billythekid

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see kogus gaa on palju ja minu parim oletus, miks, on see, et peräädikhappe valmistamine kohapeal (reaktsiooni ajal) ja ilma katalüsaatorita on ebaefektiivne, nii et keemik kompenseerib seda üle, et aidata seda, samuti kasutatakse siin lahustina GAA-d.
valmistades peräädikhapet päevi enne ja katsetades olemasoleva hapniku sisaldust, saate tõenäoliselt paremaid tulemusi. Seda öeldes olen näinud, et professionaalid kasutavad seda meetodit ja saavad parimal juhul vaid 35-65% valmistoodangust. nii et kogenematu keemik saab tõenäoliselt veelgi halvema tulemuse ja uustulnuk tõenäoliselt ebaõnnestub või veel hullemini vigastab ennast. Soovitan lugeda ja õppida ning alustada väikselt
veenduge, et puhastate oma valmis reaktsioonisegu iga sammu lõpus põhjalikult, ärge ületage aldol-kondensaatoris -5c laske mek/bensaldehüüdi segada üleöö külmkapis pärast gaasitamist.
ärge ületage 60c Bayeri küllap. ja uurige teisi oksüdeerijaid, sest ma saan paremaid tulemusi teistsuguse oksüdeerijaga.
 
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TheNut22

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Või kas ma võin kasutada jäääädikhapet oma MPB lahusena ka oma performiinhappega?
 

Grubby

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Eh3YM0zIPF
RjQlvu3DaR

Ya!ψ(`∇´)ψ RM pärast reaktsiooni bensaldehüüd + MEK + HCI muutub mustaks ja vaidlustab 3-metüül-4-fenüül-3-buten-2-ooni destillatsiooni, mille keemistemperatuur on 269! See on esimene kord, kui ma ostsin -60kpa vaakumpumba vaakumdekompressiooniks ja sain edukalt kuldkollast vedelikku 3-Metüül-4-fenüül-3-buten-2-oon! Aga masin tundub olevat ülekuumenenud. Nüüd võin ainult destilleerimise peatada... Tahate ju, et ülejäänud rm oleks täielikult destilleeritud? Ma ei taha destilleerida välja kõrgema keemistemperatuuriga lisandeid ja rikkuda oma rasket tööd⋯
 
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Labchef

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Pls show your vacuum pump and how you used it in distillation please.
 

handle

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26. oktoober 2024.
Üks meetod ütleb, et Chill and Ice MPB
Teine meetod ütleb, et Heat and Reflux MPB
Ma lihtsalt teen mõlemat :rolleyes:?
 

Labchef

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Nii et te kuumutate ja tagasilöögi MPB lahust, seejärel jahutate jääl, kas te saate kristalle, kui te seda teete ja kas kristallid on toatemperatuuril kuivad.
 

TheNut22

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Mulle ei meeldi midagi gaasida, sest minu piirkonnas on kontsentreeritud väävelhape keelatud. Ma olin nii kergendunud, kui ma sain väga häid tulemusi, et võtsin lihtsalt koostisained mõõtu, panin kogu kupatuse kokku, hakkasin kuumutama ja vaatasin filmi.
 

TheNut22

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Performiinhappe protseduur oli nagu õudusfilmi vaatamine koos vastiku paanikahooga. Kui ma lahkusin sigaretti suitsetama (4-5 min) ja tulin tagasi sisse, oli kolb nii kuum, et näis, nagu oleks see veidi keenud! Aaannnd, jälle VÄGA kiiresti jääkülma vee all ... Pärast pikka segamisprotsessi (~3,5 h) ja kuna pidin seda tegema kätega (higistades ja raputades), sest 1 L kolb ei mahu minu küttepoti külge, jätsin selle jahedasse vette. Ma olin šokeeritud, kui lugesin, et see võib toatemperatuuril bensaldehüüdiga plahvatada! Võimalik, et seal ON ka puhastatud, kuid mitte destilleeritud toode. Noh, mul on hea meel, et segu on nüüd ruumis, kus temperatuur on alla 20 C...
 

handle

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😆 selleks ongi tuleteemant.
3 = vedelikud, mida saab süüdata peaaegu kõikides keskkonnatemperatuuritingimustes
 

TheNut22

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Noh, mul õnnestus ja hea! Ja hea on õppida midagi uut keemia kohta, aitäh, ja, ütleme nii: Palju õnne...
Kuidas ma võin oma munni kondensatorisse topida ja samal ajal teha vaakum "destillatsiooni"...
 

B APPLE

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Teacher! Can you teach me how to synthesize methamphetamine from phenylacetone? Thank you
 

B APPLE

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Excuse me! I poured methylphenylbutenone with acetic acid and 50% hydrogen peroxide Is it normal for the temperature to rise to 8-90 degrees on its own?
 

Labchef

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What’s the color of your mixed MPB + acetic+ peroxide solution? I used commercial available peracetic acid. Solution color is dark brown but no rise temperature until heat was applied
 

B APPLE

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I have now completed the production of phenoxyphenylpropene!
 

B APPLE

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I saw that the teacher taught me to extract with chloroform. When I poured 800ml of chloroform down without layering, I was completely dumbfounded and spent a lot of material costs And the more I thought about it, the more unwilling I was to accept that after pouring chloroform and replacing it with DCM, the layers actually separated before using vacuum distillation to obtain it!
 

B APPLE

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Let me tell you something interesting! I bought Diethyl Phenylacetate CAS20320-59-6 and easily obtained Phenylacetone. I obtained approximately 650ml of Phenylacetone from 1000ml of Diethyl Phenylacetate! Then I watched a video on the forum and wanted to purify phenylacetone! I mixed potassium carbonate with distilled water and phenylacetone, and the whole thing kept boiling! I want to say it's too bad to be reimbursed, but after boiling over 650, there's still 180 left But it's because of this that I know it's very pure! I don't understand chemistry very well, so sometimes I ask some basic questions but nobody pays attention! They have been using materials and testing themselves all along!
 

B APPLE

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We are synthesizing more phenylacetone! I tried to synthesize methamphetamine from sodium borohydride but failed! The reason may be that the percentage of methylamine water is not high
 

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Labchef

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Can you share how you synthesize phenylacetone using diethyl phenylacetate. Is diethyl phenylacetate commercially available?
 

handle

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Diethyl phenylacetate is the same as PAA
 

B APPLE

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I bought it on Alibaba in mainland China
 

B APPLE

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Diethyl styrene malonate CAS: 20320-59-6. I watched Mr. Barton use 55.66 grams of diethyl phenylacetylmalonate, 7.5 ml of sulfuric acid, 40 ml of acetic acid, and 60 ml of distilled water to heat and reflux for 4-5 hours. Then, extract 50 ml of the combined solution three times with ether, wash with 200 ml of water, and remove the water with sodium sulfate before vacuum distillation
 
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