Videosinteza 1-fenil-2-nitropropena (P2NP) iz benzaldehida in nitroetana. Henryjeva reakcija.

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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Ali lahko vem, ali je nitrometan enak nitroetanu?

In ali je mogoče ta element (kot je priložena zaslonska slika) uporabiti kot n-butilamin? Če je odgovor pritrdilen, kako bi predlagali, da ravnam?
 

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William D.

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Ne, to so različni reagenti. Z nitrometanom bomo dobili nitrostiren. Nitrometan z nekaterimi substituiranimi benzaldehidi je primeren za sintezo virov velikega razreda snovi, različnih psihedelikov.
Ne
 
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Montecristo

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Kakšen je izkoristek pri toplotni metodi?
 

William D.

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pred 1,5 kg
 
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cyb3r0

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Prijatelj, nitroetana nikoli ne moremo dobiti, ali v tem primeru obstaja alternativa zanj?
 

HIGGS BOSSON

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Težave z nitroetanom v Evropi so se začele že leta 2007, nato pa so postopoma vse države uvedle omejitve za ta dragoceni reagent. In zdaj sta na voljo dve možnosti: poiskati dobavitelje v državah s šibko zakonodajo z razvito kemijsko industrijo, na primer v Bangladešu, ali samostojno sintetizirati, metodologijo za to smo predlagali.
 

Alojz

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S čim lahko nadomestimo ali sintetiziramo nitroetan?
 

Kvadprime

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You can find methods of syntes nitroethane in another thread
 

anotherNovice

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Najdem benzaldehid za parfumerijo z oznako CAS 100-57-2. Ali je to isto kot zahtevano?
 

mactipo01

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Pozdravljeni!
kaj je ipa?
in koliko metanfetamina lahko dobim s postopkom?
ty beforhand :)
 

ActionAyi

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Izopropilalkohol, znan tudi kot 2-propan-ol
 

mactipo01

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kje lahko kupim 10l bučko?
 

HIGGS BOSSON

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V tej temi je objavljena metoda za pridobivanje fenilnitropropena, predhodnika za sintezo amfetamina. Če potrebujete metamfetamin, si oglejte ustrezne teme. IPA - izopropilni alkohol

 
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mactipo01

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oh ty!!!.. zelo lepo....je zelo težko naučiti to...in ni enostavno to narediti.
ti morda
prodajate? ali veste, kje lahko kupim kakšne stimulativne tablete?
 

William D.

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V zvezi s to temo vam lahko pomagamo pri sintezi P2NP. Druge razprave v drugih temah
 

mactipo01

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Oprostite, sem novinec... kaj je preprosta metoda za sintezo metamfetamina? P2NP ali iz tablet efedrina?
 

William D.

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P2NP/Al/Hg, dobra pot za začetek, vendar težavna za velike razsežnosti
 
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a_king

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kako dobiti n-butilamen prosim
 

William D.

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u lahko zamenjate za cikloheksilamin
 

Macondor

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Heksametilentetramin se lahko uporabi za piperon za MDP2NP?
 

ASheSChem

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Pozdravljeni;
če uporabimo cikloheksilamin, ali potrebujemo ledeniško ocetno kislino ?
 
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