Síntese em vídeo de 1-fenil-2-nitropropeno (P2NP) a partir de benzaldeído e nitroetano. Reação de 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).
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tankikan

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Posso saber se Nitromethane é igual a nitroethane?

E é possível usar esse item (conforme captura de tela anexa) como n-butilamina? Em caso afirmativo, como você sugeriria proceder?
 

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MisterAnonymous

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Envie-me um DM que eu lhe fornecerei um contato para nitroetano e N-butilamina...
 

William D.

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Não, esses são reagentes diferentes. Com nitrometano, obteremos nitroestireno. O nitrometano com alguns benzaldeídos substituídos é adequado para a síntese das fontes de uma grande classe de substâncias, várias psicodélicas.
Não
 
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Montecristo

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Qual é o rendimento do método de calor?
 

William D.

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antes de 1,5 kg
 
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cyb3r0

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Meu amigo, nunca conseguimos nitroetano, existe alguma alternativa para ele nesse caso?
 

HIGGS BOSSON

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Os problemas com o nitroetano na Europa começaram em 2007 e, gradualmente, todos os países impuseram restrições a esse valioso reagente. E agora há duas maneiras: procurar fornecedores em países onde há uma legislação fraca com um setor químico desenvolvido, por exemplo, Bangladesh, ou sintetizar de forma independente, a metodologia que propusemos para isso.
 

Alojz

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O que pode ser usado para substituir ou sintetizar o nitroetano?
 

Kvadprime

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You can find methods of syntes nitroethane in another thread
 

anotherNovice

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Posso encontrar benzaldeído para perfumaria rotulado como CAS 100-57-2. É o mesmo que o exigido?
 

mactipo01

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Olá!!!
o que é ipa?
e qual a quantidade de metanfetamina que posso obter com o processo?
Obrigado :)
 

ActionAyi

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Isopropylalcohol também conhecido como 2-propane-ol
 

mactipo01

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Onde posso comprar um frasco de 10 litros?
 

HIGGS BOSSON

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Neste tópico, é publicado um método para obter fenilnitropropeno, um precursor para a síntese de anfetamina. Se você precisar de metanfetamina, consulte os tópicos relevantes. IPA - álcool isopropílico

 
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mactipo01

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oh ty!!!... muito bom....é muito difícil aprender isso... e não é simples fazê-lo.
talvez você
ou sabe onde posso comprar algumas pílulas estimulantes?
 

William D.

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Com relação a esse tópico, podemos ajudar com a síntese de P2NP. Outras discussões em outros tópicos
 

mactipo01

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desculpe, sou novato... qual é o método simples para sintetizar metanfetamina? P2NP ou a partir de comprimidos de efedrina?
 

William D.

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P2NP/Al/Hg, boa rota para começar, mas difícil para grandes escalas
 
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a_king

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como obter o n-butilâmen por favor
 

William D.

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u pode substituir cyclohexylamine
 

Macondor

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A hexametilenotetramina pode ser usada como piperonal para MDP2NP?
 

ASheSChem

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Olá, pessoal;
Se usarmos ciclohexilamina, precisaremos de ácido acético glacial?
 
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