Phenylacetone (P2P) synthesis from benzaldehyde with butanone

[cokemuffin]

I would say DCM, but I might be wrong
You also easily make chloroform by reacting cold 0* C bleach with acetone in stoechiometric amounts with a small 10% ish molar excess of bleach.Nilered has a video.

UWe9o12jkied91dI saw the video, but i'm mainly interested in large scale manufacture, getting 6l chloroform that way is not really cheap and efficient. I'll probably try to further chlorinate DCM to chloroform.

 

[Sneaky.Base]

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[jokerr]

Im running the same process at the same stage. Don't expectuch help from the team here. They seem to have abandoned this write up. I think a lot of write ups are just copy pasted.




Consider, that MEK and Benzaldehyde have different molecular weight and density. Therefore 100ml of MEK is not 100g. This only an issue later when you go to add 100g of h202(50%)

There are several measures in this write up where one side of the reaction is stated in grams and the other in MLS. H2O2 I stated in grams of a 50/50 mixture. So you have to account for the water and the peroxide when calculating the MLS from weight. Unless your going to start weighing liquids.

Let me know how you go, when I did .1M reaction I ended up with such poor yields that i couldn't extract the p2p from the tar crap. This write up doesn't really inform you much along the way of what to expect. You can the impression of just extract and distill.

Let me know how you go extracting the MPB tomorrow. Did your Rx mixture go bright red?

FensterI realized my mistake.
thanks a lot by faster

 

[Fenster]

I realized my mistake.
thanks a lot by faster

jokerrI ended up with a very very dark organic layer with DCM. I then distilled this under vacuum which removed the DCM and then a yellow oil came over. This was frozen overnight and the first time needed to be manipulated to crystal, second time was 60g solid xtal mass sulfur coloured and smelling of camphor.

 

[Fenster]

@jokerr I don't think gpatton is interested. I asked for soooo much help and they seemed to just wait until I got frustrated and then disarming language by accusing me of not following procedure. I've have DM the op and no response.

I have the original forensics write up. Might shed some light. This write up is honestly dog shit here.

 

[G.Patton]

The solution is extracted with chloroform (CHCl3) 800 ml x2, then the extract is washed with sodium bicarbonate solution (NaHCO3) to neutral pH

Are there two different operations in order of what I need to do in this section?

jokerrHi. It means that you have to combine extracts, add aqueous NaHCO3 solution and extract it (yes liquid / liquid extraction), then separate layers. You have to check pH of organic solution after this procedure. It have to be neutral (pH 6.5-7.5).

 

[panchaspsycho]

Hello I have a question. Everything is clear but how do you heat that gigantic thing to 55° or reaction+stirring at high speed will generate heat itself?

 

[G.Patton]

Hello I have a question. Everything is clear but how do you heat that gigantic thing to 55° or reaction+stirring at high speed will generate heat itself?

panchaspsycho

Laboratory FAQ==>Reflux and heating techniques​

 

[Mo0odi]

Hydrogen peroxide (H2O2) 1300 g 50 %;

William DampierIs there an alternative to peroxide hydrogen ?

 

[Ortist]

Is there an alternative to peroxide hydrogen ?

Mo0odiOriginal twodogs procedure uses perboric acid made in-situ from acetic acid & sodium perborate. Perboric route is a bit messy and requires filtering

 

[TheNut22]

Original twodogs procedure uses perboric acid made in-situ from acetic acid & sodium perborate. Perboric route is a bit messy and requires filtering

OrtistI used one time performic acid, and it worked, but not as well as peracetic acid.

 

[Mo0odi]

We can provide hydrogen peroxide but with a concentration of 6%

 

[Slayer]

Can we use magmetic stirer with heating function and flask as a batch reactor or any alternative for batch reactor ?

 

[Riot]

Have good day ı have question ı want to m ake small rate of synthes , is there alternative for batch reactor and can ı use acetic asid %99 as a glacial acetic asid thank you

 

[G.Patton]

Have good day ı have question ı want to m ake small rate of synthes , is there alternative for batch reactor and can ı use acetic asid %99 as a glacial acetic asid thank you

RiotHello, this is same

can ı use acetic asid %99 as a glacial acetic asid

Yes, you can use three-necked round bottom flask

is there alternative for batch reactor

 

[Riot]

Hello, this is same

Yes, you can use three-necked round bottom flask

G.PattonThanks patton

 

[Riot]

Hello, this is same

Yes, you can use three-necked round bottom flask

G.PattonPatton ı have magnetic stirer with heater how can ı properly heat my round bottom flask ?

 

[G.Patton]

Patton ı have magnetic stirer with heater how can ı properly heat my round bottom flask ?

RiotDear Riot, read Laboratory FAQ section please.

 

[the money]

Is there a video about the synthesis of P2P from benzaldehyde

 

[Riot]

Reagents:​

• Benzaldehyde 1000 g;​
• Methyl ethyl ketone (MEK) 1000 ml;​
• Distilled water 14.5 L;​
• Chloroform (CHCl3) 7.6 L;​
• Sodium bicarbonate solution (NaHCO3);​
• Magnesium sulphate (Na2SO4) anhydrous;​
• Glacial acetic acid 10 L;​
• Hydrogen peroxide (H2O2) 1300 g 50 %;​
• Sodium hydroxide (NaOH) 600 g;​

Equipment and glassware:​

• 5 and 10 L Round bottom flasks;​
• Water bath;​
• HCl gas source;​
• 25-30 L Batch reactor with reflux condenser and heating system;​
• Vacuum source;​
• Glass rod and spatula;​
• Rotovap machine (optional);​
• pH indicator paper;​
• Laboratory scale (1-1000 g is suitable);
• Measuring cylinders 1000 mL;
• 1000 mL x3; 2000 mL x3; 5000 mL x3 Beakers;
• Several buckets;

Step 1. 3-Methyl-4-phenyl-3-buten-2-one synthesis (cas 1901-26-4).
1. Benzaldehyde 1000 g and methyl ethyl ketone (MEK) 1000 ml are mixed in 5 L flask, stirred and chilled at 0 °C.
2. HCl gas is bubbled slowly through the mixture for a 1.5 h.
3. The solution is stirred for addition 1.5 h at room temperature.
4. Distilled water 2 L is added. The solution is extracted with chloroform (CHCl3) 800 ml x2, then the extract is washed with sodium bicarbonate solution (NaHCO3) to neutral pH and dried over magnesium sulphate (MgSO4).
5. Solvent is evaporated under vacuum and 3-methyl-4-phenyl-3-buten-2-one (cas 1901-26-4) is distilled under vacuum (b.p. 269.6±9.0 °C at 760 mm Hg). Reaction yield is 1000 g.​

View attachment 1386
​

Step 2. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) synthesis.

1. 3-Methyl-4-phenyl-3-buten-2-one (cas 1901-26-4) 1 kg from Step 1, glacial acetic acid 10 L and hydrogen peroxide (H2O2) 1300 g 50 % are poured into a 25-30 L batch reactor with reflux condenser, stirred and at 55 °C for 23 h.
2. Next, distilled water 10 L is added.
3. The reaction mixture is extracted with chloroform 5 L and dried over magnesium sulphate (Na2SO4).
4. Solvent is evaporated under vacuum. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) yield is 800 g.​

View attachment 1387​

Step 3. 1-Phenyl-2-propanone (P2P; cas 103-79-7).

1. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) 800 g from Step 2 and sodium hydroxide (NaOH) 600 g in distilled water 2500 ml is stirred at 50 °C for 12 h in 10 L flask with reflux condenser.
2. Reaction solution is extracted with chloroform 1000 ml, dried over magnesium sulphate (Na2SO4) and the solvent is evaporated under vacuum. 1-Phenyl-2-propanone yield is 650 g.​

View attachment 1388​

William DampierI need some help.
does heptahydrate Na2SO4 will do the work as anhydrous ?
can ı drop hcl over the time of 1.5 or hcı is necessary in this reaction
ın step1 1. we chilled in 0 degree using water bath and then we flow hcl gas or remove water bath and then flow hcl

thanks.

 

[Riot]

I need some help.
does heptahydrate Na2SO4 will do the work as anhydrous ?
can ı drop hcl over the time of 1.5 or hcı is necessary in this reaction
ın step1 1. we chilled in 0 degree using water bath and then we flow hcl gas or remove water bath and then flow hcl

thanks.

Riot*edit*
hcı gas necessary in this reaction ?

 

[Sneaky.Base]

This method looks awesome, otc cheap chemicals.
Why expensive dcm while chloroform exists. If you want a long time coock you ll understand making chloroform is the job you have to do.
The write up method shared here is perfect, it shows it written by a professional . I ll wonder if there are any video a bout this method. Tnx for sharing this nice write up willi

 

[Mo0odi]

This method looks awesome, otc cheap chemicals.
Why expensive dcm while chloroform exists. If you want a long time coock you ll understand making chloroform is the job you have to do.
The write up method shared here is perfect, it shows it written by a professional . I ll wonder if there are any video a bout this method. Tnx for sharing this nice write up willi

Sneaky.BaseI support your words