Video sintesi dell'1-fenil-2-nitropropene (P2NP) da benzaldeide e nitroetano. Reazione di Henry.

GhostChemist

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Equipment and glassware:
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Reagents:
  • Benzaldehyde 1000 ml;
  • Nitroethane 1000 ml;
  • Glacial acetic acid 250 ml;
  • n-Butylamine 50 ml;
  • Isopropyl alcohol (IPA) ~1000 ml;
Medium scale:
1. Benzaldehyde 1000 ml, nitroethane 1000 ml, glacial acetic acid 250 ml and n-butylamine 50 ml are placed into 10 L flask.
2. A reflux condenser is installed onto the flask.
3. The stirrer and heater are turned on. The reaction mixture is heated up to 60 °С.
4. The reaction is conducted during 2-3 hours with constant stirring at 60 °С.
5. The reaction mixture is poured into an empty 5-10 L bucket.
6. Isopropyl alcohol (IPA) 800 ml is poured into the bucket and stirred.
7. The bucket with mixture is put into a freezer for 12 hours, 1-phenyl-2-nitropropene (
P2NP) is crystallized.
8. The product P2NP is filtered on a Buchner funnel (
suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).
The yield is 65-75%.



Equipment and glassware:
  • Beaker 500 ml;
  • Funnel;
  • Vacuum source;
  • Laboratory scale (0.1-500 g is suitable) - optional;
  • Measuring cylinders 50 mL and 100 mL;
  • Glass rod and spatula;
  • Filter paper;
  • Buchner flask and funnel;
  • Freezer;
  • Microwave oven 750 W;
Reagents:
  • Benzaldehyde 100 ml;
  • Nitroethane 100 ml;
  • Glacial acetic acid 25 ml;
  • n-Butylamine 20 ml;
  • Isopropyl alcohol (IPA) ~150 ml;

Microwave (small) scale:
1. Benzaldehyde 100 ml, nitroethane 100 ml, glacial acetic acid 25 ml and n-butylamine 20 ml are placed into 500 ml beaker.
2. A rubber glove is put onto the beaker.
3. The beaker is put into a microwave oven.
4. The power of the microwave oven is set up on 750 W. Oven is turned on and the mixture is warmed until the boiling. The mixture is cooled down to the room temperature.
5. Step 4 is repeated several times. Minimum 6 times.
6. Next, IPA 100 ml is added, reaction mixture is stirred and put into a freezer for 12 hours. 1-Phenyl-2-nitropropene (
P2NP) is crystallized.
7. The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).

1-Phenyl-2-nitropropene (P2NP) recrystallization

1-Phenyl-2-nitropropene (P2NP) can be recrystallized from hexane, methanol, ethanol or isopropanol (IPA).
Download Video
 
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tankikan

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Posso sapere se il nitrometano è uguale al nitroetano?

Ed è possibile utilizzare questo elemento (come da schermata allegata) come n-butilammina? Se sì, come suggerite di procedere?
 

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MisterAnonymous

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Inviatemi un DM che vi fornirò un contatto per il nitroetano e la N-butilammina...
 

William D.

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No, si tratta di reagenti diversi. Con il nitrometano si ottiene il nitrostirene. Il nitrometano con alcune benzaldeidi sostituite è adatto alla sintesi delle fonti di un'ampia classe di sostanze, vari psichedelici.
No
 
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Montecristo

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Qual è il rendimento del metodo del calore?
 

William D.

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prima di 1,5 kg
 
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cyb3r0

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Amico mio, non riusciamo mai a procurarci il nitroetano, c'è un'alternativa in questo caso?
 

HIGGS BOSSON

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I problemi con il nitroetano in Europa sono iniziati nel 2007, poi gradualmente tutti i Paesi hanno imposto restrizioni su questo prezioso reagente. Ora ci sono due strade: cercare fornitori in Paesi con una legislazione debole e un'industria chimica sviluppata, come ad esempio il Bangladesh, oppure sintetizzare autonomamente, con la metodologia che abbiamo proposto.
 

Alojz

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Cosa si può usare per sostituire o sintetizzare il nitroetano?
 

Kvadprime

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You can find methods of syntes nitroethane in another thread
 

anotherNovice

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Riesco a trovare la benzaldeide per la profumeria con l'etichetta CAS 100-57-2. È la stessa cosa richiesta?
 

mactipo01

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ciao!
cos'è l'ipa?
e quanta metanfetamina posso ottenere con il processo?
ty beforhand :)
 

ActionAyi

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Alcool isopropilico noto anche come 2-propane-olo
 

mactipo01

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dove posso acquistare un pallone da 10l?
 

HIGGS BOSSON

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In questo argomento viene pubblicato un metodo per ottenere il fenilnitropropene, un precursore per la sintesi dell'anfetamina. Se avete bisogno di metanfetamina, consultate gli argomenti pertinenti. IPA - alcool isopropilico

 
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mactipo01

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oh ty!... molto bello.... è molto difficile imparare questo... e non è semplice farlo.
forse
vendere? o sapere dove posso comprare delle pillole stimolanti?
 

William D.

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Per quanto riguarda questo argomento, possiamo aiutarvi con la sintesi di P2NP. Altre discussioni in altri argomenti
 

mactipo01

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Scusate, sono nuovo... qual è il metodo semplice per sintetizzare la metanfetamina? P2NP o dalle compresse di efedrina?
 

William D.

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P2NP/Al/Hg, una buona strada per iniziare ma difficile per le grandi scale
 
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a_king

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come ottenere il n-butilamen per favore
 

William D.

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u può sostituire alla cicloesilammina
 

Macondor

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L'esametilentetramina può essere utilizzata per il piperonale a MDP2NP?
 

ASheSChem

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ciao ragazzi;
se usiamo la cicloesilammina, abbiamo bisogno di acido acetico glaciale?
 
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