Video Síntesis de 1-fenil-2-nitropropeno (P2NP) a partir de benzaldehído y nitroetano. Reacción 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).
Download Video
 
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tankikan

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¿Puedo saber si el nitrometano es igual al nitroetano?

¿Y es posible utilizar este elemento (como la captura de pantalla adjunta) como n-butilamina? En caso afirmativo, ¿cómo sugiere que procedamos?
 

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MisterAnonymous

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Envíeme un DM Le facilitaré un contacto para nitroetano y N-butilamina...
 

William D.

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No, se trata de reactivos diferentes. Con nitrometano, obtendremos nitrostireno. El nitrometano con algunos benzaldehídos sustituidos es adecuado para la síntesis de las fuentes de una gran clase de sustancias, varios psicodélicos.
No
 
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Montecristo

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¿Cuál es el rendimiento del método térmico?
 

William D.

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antes de 1,5 kg
 
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cyb3r0

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Amigo mío, nunca podemos conseguir nitroetano, ¿hay alguna alternativa en este caso?
 

HIGGS BOSSON

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Los problemas con el nitroetano en Europa empezaron en 2007, y poco a poco todos los países fueron imponiendo restricciones a este valioso reactivo. Y ahora hay dos caminos: buscar proveedores en países donde la legislación es débil con una industria química desarrollada, por ejemplo, Bangladesh, o sintetizarlo de forma independiente, metodología para la que hemos propuesto un método.
 

Alojz

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¿Qué puede utilizarse para sustituir o sintetizar el nitroetano?
 

Kvadprime

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You can find methods of syntes nitroethane in another thread
 

anotherNovice

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Puedo encontrar benzaldehído para perfumería con la etiqueta CAS 100-57-2. ¿Es lo mismo que se requiere?
 

mactipo01

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¡¡¡hola!!!
¿qué es la ipa?
y ¿cuánta metanfetamina puedo obtener con el proceso?
ty beforhand :)
 

ActionAyi

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Alcohol isopropílico también conocido como 2-propane-ol
 

mactipo01

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¿dónde puedo comprar frascos de 10 l?
 

HIGGS BOSSON

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En este tema, se publica un método para obtener fenilnitropropeno, un precursor para la síntesis de anfetamina. Si necesita metanfetamina, consulte los temas correspondientes. IPA - alcohol isopropílico

 
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mactipo01

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oh ty!!.. muy bonito....es muy difícil aprender esto... y nada sencillo hacerlo.
¿quizás
lo vendes? o sabes donde puedo comprar algunas pastillas estimulantes?
 

William D.

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En relación con este tema, podemos ayudarle con la síntesis de P2NP. Otras discusiones en otros temas
 

mactipo01

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lo siento, soy nuevo... ¿cuál es el método sencillo para sintetizar metanfetamina? ¿P2NP o a partir de pastillas de efedrina?
 

William D.

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P2NP/Al/Hg, buena ruta para empezar pero difícil para grandes escalas
 
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a_king

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cómo conseguir n-butilamen por favor
 

William D.

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u puede sustituir a ciclohexilamina
 

Macondor

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¿Puede utilizarse la hexametilentetramina para el piperonal a MDP2NP?
 

ASheSChem

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hola chicos
si utilizamos ciclohexilamina, ¿necesitamos ácido acético glacial?
 
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