1-Phenyl-2-nitropropene (P2NP) Video Synthesis From Benzaldehyde and Nitroethane. Henry Reaction.

[Hank Schrader]

When we produced phenylnitropropene, we did not use heating.
Poured into a flask
nitroethane+benzaldehyde+catalyst was closed and left at room temperature.
The flask was shaken once a day. After 8 days, the solution was poured into water ... and propene crystals fell immediately to the bottom. The water was decanted and crystallized in alcohol.

If someone wants to get very high quality propene,
I will give you the technology below:

1 mole benzaldehyde
1,2 mole of nitroethane
+ 18ml n-butylamine

Put this in a glass bottle and close it.
Shake hard a couple of times a day.
After 8 days, open the bottle and pour 1 liter into a container of hot water.
Shake... drain the water, repeat the procedure with 500 ml of water.
Pour phenylnitropropene with alcohol and heat until completely dissolved and leave in the freezer.
Propene is obtained by this method practically without color.
The color is transparent yellow, the structure is like crystal methamphetamine.

According to my method, it will turn out ~ 135-140g

 

[Akashic]

When we produced phenylnitropropene, we did not use heating.
Poured into a flask
nitroethane+benzaldehyde+catalyst was closed and left at room temperature.
The flask was shaken once a day. After 8 days, the solution was poured into water ... and propene crystals fell immediately to the bottom. The water was decanted and crystallized in alcohol.

If someone wants to get very high quality propene,
I will give you the technology below:

1 mole benzaldehyde
1,2 mole of nitroethane
+ 18ml n-butylamine

Put this in a glass bottle and close it.
Shake hard a couple of times a day.
After 8 days, open the bottle and pour 1 liter into a container of hot water.
Shake... drain the water, repeat the procedure with 500 ml of water.
Pour phenylnitropropene with alcohol and heat until completely dissolved and leave in the freezer.
Propene is obtained by this method practically without color.
The color is transparent yellow, the structure is like crystal methamphetamine.

According to my method, it will turn out ~ 135-140g

Hank Schraderwhen shaking initial solution daily 8 days at room temp, will the capped flask need to be vented? and should the rv avoid light exposure? I imagined I would choose a large amber media bottle and store in cupboard before it’s time to wash/xtaled
thanks for sharing Id really like to try your method

 

[41Dxflatline]

when shaking initial solution daily 8 days at room temp, will the capped flask need to be vented? and should the rv avoid light exposure? I imagined I would choose a large amber media bottle and store in cupboard before it’s time to wash/xtaled
thanks for sharing Id really like to try your method

BigjohnsonMy avatar is a large crystal from this method, magnified

 

[JustMe]

Can I replace Cyclohexylamine ?
Benzaldehyde 50 ml
Nitroethane 50 ml
Glacial acetic acid 20 ml
aqueous methylamine 10 ml

 

[G.Patton]

Can I replace Cyclohexylamine ?
Benzaldehyde 50 ml
Nitroethane 50 ml
Glacial acetic acid 20 ml
aqueous methylamine 10 ml

JustMeHello, can you clarify your question please? What do you want to replace exactly?

 

[G.Patton]

*My English is weak

see thes
[Phenyl-2-Nitropropene à la Barium: 1 mol benzaldehyde, 1.2 mol nitroethane and 15 mL diluted aqueous methylamine in 150 mL alcohol. Stirred and slightly heated for ca 4 hours. The reaction mixture is brought over into a beaker and cooled in the fridge (4°C). If precipitation doesn't commence at this point, water is poured in and the mixture put back in the fridge. The P2NP oil layer will slowly (or sometimes quickly) start forming a crystalline layer. If it doesn't, scratching the wall with e.g. a glass rod will help. If even this won't help, it means you probably fucked something up. The yields I have had using this "adaptation": 81% (i-PrOH), 79% (i-PrOH), 75% (EtOH) and 71% (EtOH) (yields calculated after crystallizing once; I store my crystals in the freezer and also recrystallize them prior to use).]

*i dont have Cyclohexylamine.

JustMe

à la Barium

Barium??

 

[JustMe]

Barium??

G.Patton

Synthesis of Phenyl-2-Nitropropene - [www.rhodium.ws]

 

[G.Patton]

Synthesis of Phenyl-2-Nitropropene - [www.rhodium.ws]

JustMeok

 

[Felix34-73]

Ammonium Acetate Catalysis in Excess Nitroethane3​

A solution of benzaldehyde (6.4 g) and ammonium acetate (1.0 g) in nitroethane (20 mL) was heated to reflux for 5 h. On cooling, after removal of the solvent, the residue was purified by column chromatography on silica gel 60 N (neutral; hexane-chloroform, 2:1, v/v), then recrystallized from hexane and gave 1-phenyl-2-nitropropene as a light yellow crystals weighing 6.2g (63%), mp 71-73°C.
Can you write the whole mole calculation for this method?

 

[BrownRiceSyrup]

Ammonium Acetate Catalysis in Excess Nitroethane3​

A solution of benzaldehyde (6.4 g) and ammonium acetate (1.0 g) in nitroethane (20 mL) was heated to reflux for 5 h. On cooling, after removal of the solvent, the residue was purified by column chromatography on silica gel 60 N (neutral; hexane-chloroform, 2:1, v/v), then recrystallized from hexane and gave 1-phenyl-2-nitropropene as a light yellow crystals weighing 6.2g (63%), mp 71-73°C.
Can you write the whole mole calculation for this method?

Felix34-73.060 mol benzaldehyde + .266 mol of nitroethane -> .038 mol of P2NP
68% of the benzaldehyde was made into P2NP

there is 4.4 times more nitroethane than benzaldehyde
hell of an excess for yield that's average at best.

im pretty sure if you add a solvent like glacial acetic acid, and instead of reflux you just heat to 60-80 you, wont need so much nitroethane and will still get similar if not slightly better yield.

Dont quote me on this part cause im not 100% sure but at reflux temps something else has a tendency to form. Anything above 100 degrees C starts to make this. all reagents here boil above 100c....

 

[BrownRiceSyrup]

.060 mol benzaldehyde + .266 mol of nitroethane -> .038 mol of P2NP
68% of the benzaldehyde was made into P2NP

there is 4.4 times more nitroethane than benzaldehyde
hell of an excess for yield that's average at best.

im pretty sure if you add a solvent like glacial acetic acid, and instead of reflux you just heat to 60-80 you, wont need so much nitroethane and will still get similar if not slightly better yield.

Dont quote me on this part cause im not 100% sure but at reflux temps something else has a tendency to form. Anything above 100 degrees C starts to make this. all reagents here boil above 100c....

BrownRiceSyrupYea and the molar ratio of whats in the video is basically 1.5 times as much nitroethane as benzaldehyde. instead of 4.44...... same amount of liquid for each but nitroethane weighs less so youre actually adding more nitro than benzaldehyde even if youre addding the same volume of each.

i know where you got that recipe btw, and looking at the other ratios on that page there are 2 other examples that uses a ratio of 1.5 Nitroethane to 1 benzaldehyde. And the rest are 1 to 1. Based on whats on that page, you can do 1:1 ratio with either cyclohexylamine or n-butylamine and be fine. As far as ammonium acetate i dont know how it compares to the larger catalysts and what ratios are optimal....

 

[Felix34-73]

Yea and the molar ratio of whats in the video is basically 1.5 times as much nitroethane as benzaldehyde. instead of 4.44...... same amount of liquid for each but nitroethane weighs less so youre actually adding more nitro than benzaldehyde even if youre addding the same volume of each.

i know where you got that recipe btw, and looking at the other ratios on that page there are 2 other examples that uses a ratio of 1.5 Nitroethane to 1 benzaldehyde. And the rest are 1 to 1. Based on whats on that page, you can do 1:1 ratio with either cyclohexylamine or n-butylamine and be fine. As far as ammonium acetate i dont know how it compares to the larger catalysts and what ratios are optimal....

BrownRiceSyrupso can you do all the molarity calculations of the ammonium acetate method? cyclohexamine is very expensive in my country so I want this method

 

[BrownRiceSyrup]

so can you do all the molarity calculations of the ammonium acetate method? cyclohexamine is very expensive in my country so I want this method

Felix34-73with the method you quoted above, like i says earlier thats basically

.060 mol benzaldehyde + .266 mol nitroethane + .012 mol ammonium acetate -> .038 mol P2NP

 

[Felix34-73]

with the method you quoted above, like i says earlier thats basically

.060 mol benzaldehyde + .266 mol nitroethane + .012 mol ammonium acetate -> .038 mol P2NP

BrownRiceSyrupI have a 1 liter balloon, can you write the maxs mole calculation?

 

[ossi]

Reaction scheme:

View attachment 1298 ​

Equipment and glassware:

• 10 L Flask;
• Retort stand and clamp for securing apparatus (optional);
• Reflux condenser;
• Funnel;
• Vacuum source;
• Laboratory scale (0.1-500 g is suitable) - optional;
• Measuring cylinders 1000 mL and 100 mL;
• Water bath;
• Glass rod and spatula;
• Filter paper;
• Laboratory grade thermometer;
• Buchner flask and funnel;
• Bucket 5-10 L.
• Freezer;

Reagents:

• Benzaldehyde 1000 ml;
• Nitroethane 1000 ml;
• Glacial acetic acid 250 ml;
• n-Butylamine 50 ml;
• Isopropyl alcohol (IPA) ~1000 ml;

Download Video

1-Phenyl-2-nitropropene synthesis

• Novator
• Apr 5, 2023
• 35
• 1-phenyl-2-nitropropene amphetamine benzaldehyde cas 100-52-7 cas 705-60-2 henry reaction nitroethane p2np p2np synthesis phenyl-2-nitropropene video synthesis

Benzaldehyde and nitroethane Henry condensation...

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).​

---

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) can be recrystallized​

GhostChemistHi,

n-Butylamin cas is 109-73-9?

 

[JohnWebb]

Hello,
In the video a 2000ml flask is used for 1950ml of liquid. The description says 10l flasks is used for 2300ml of liquid. May I ask why so big flask?
Isn't it possible to use a smaller flask in this quantity?

 

[Marvin "Popcorn" Sutton]

Hello,
In the video a 2000ml flask is used for 1950ml of liquid. The description says 10l flasks is used for 2300ml of liquid. May I ask why so big flask?
Isn't it possible to use a smaller flask in this quantity?

JohnWebbYes, the 10-liter flask can be filled with more volume than the methodology states. But I still recommend using 1/2 or 2/3 of the volume of the flask. If the reaction mixture comes to a strong boil, it may foam, and the contents of the flask will pour out.

 

[JohnWebb]

Yes, the 10-liter flask can be filled with more volume than the methodology states. But I still recommend using 1/2 or 2/3 of the volume of the flask. If the reaction mixture comes to a strong boil, it may foam, and the contents of the flask will pour out.

Marvin "Popcorn" SuttonThank you very much for your reply

 

[MrMarvin]

Which Thermometer should i buy guys?
In need one that is very suitable in the Amphetamine Synthesis too
Is an Infrared suitable??

 

[41Dxflatline]

Which Thermometer should i buy guys?
In need one that is very suitable in the Amphetamine Synthesis too
Is an Infrared suitable??

MrMarvinA proper glass thermometer is better because you will need one for distillation set ups anyway. can get them in ranges that go below zero and above 200C for cheaper than a infrared hand held one.

Joke answer: Bulk pack of mercury thermometers so you can break them open

 

[yuiopjkl]

I can't get cyclohexylamine nor butylamine but I can get ammonium acetate.
I'm going to do 100ml benzaldehyde, 100ml nitroethane and 25ml acetic acid.
So how much ammonium acetate will I need?

 

[41Dxflatline]

I can't get cyclohexylamine nor butylamine but I can get ammonium acetate.
I'm going to do 100ml benzaldehyde, 100ml nitroethane and 25ml acetic acid.
So how much ammonium acetate will I need?

yuiopjklWhy can't you get them?

 

[yuiopjkl]

Why can't you get them?

41DxflatlineIt is not available locally, and if you order it online, it will take more than a month to get here.
ammonium acetate i can get it today

 

[yuiopjkl]

Hello. Well, ammonium acetate work as other Lewis bases (like cyclohexylamine and butylamine). So, you have to take about 4 g in accordance with approximate molar ratio. I'm not sure in this amount. It's worth to check in smaller scale synthesis batch like 10g load.

G.PattonHow much ammonium acetate and GAA do I need to add to
10g benzaldehyde and
10g nitroethane

thanks in advance

 

[G.Patton]

How much ammonium acetate and GAA do I need to add to
10g benzaldehyde and
10g nitroethane

thanks in advance

yuiopjklyou can reduce amounts proportionally