Synthesis of 4-methylpropiophenone from toluene by Friedel-Crafts reaction (1kg+ scale)

[Oxygen]

There was a alternative for mechanical stirrer?

 

[HectorFromTroy]

There was a alternative for mechanical stirrer?

OxygenOne Alternative would be strong magnetic stirrer although the large ones are pretty pricy and it would be more cost effective to buy a mechanical one.

 

[Deedubbau]

For example, what is the alternative ??? The volume of the reaction mass is approximately 5.5 liters, then the reactor is at least twice as large. Substances are extremely aggressive. I don't see any alternative. It is necessary to use a reactor (stainles steel) with a mechanical stirrer and a flue gas for synthesis. Protective suit (full body) with boots and gloves and a gas mask (complete head). It is also necessary to take into account the large amount of heat generated during the reaction.

Hans-Dietrich
Mr. Safety to the rescue....

Yeah you better make sure you are wearing all that protective gear. Cause if you take this advise and use stainless steel you are going to have a disaster on your hands. Stainless is rapidly attacked by organic acids, and chlorides. So once you warm this mix up you better be prepared to run....or just stick with glass

 

[The-Hive]

Mr. Safety to the rescue....

Yeah you better make sure you are wearing all that protective gear. Cause if you take this advise and use stainless steel you are going to have a disaster on your hands. Stainless is rapidly attacked by organic acids, and chlorides. So once you warm this mix up you better be prepared to run....or just stick with glass

DeedubbauI use stainless steel vessel for larger reactions so far so good IMO

 

[estimated]

hello, can toluene be replaced with xylene?

 

[plancklong]

hello, can toluene be replaced with xylene?

estimatedNo. The toluene is not just the solvent. It is the basis for the 4-methylpropiophenone:

Which xylene did you have in mind, o, m, or p? Never mind, it's probably a mixture of all 3:

If you did use these, can you see that you would NOT be synthesizing 4-methylpropiophenone?

 

[HectorFromTroy]

hello, can toluene be replaced with xylene?

estimatedYou could synthesise toluene from xylene by hydrogenation although toluene is pretty easy to source therefore doing this isn’t that practical.

 

[reza]

Does it mean I don't heat? Don't you think it will take a long time to completely evaporate?
Thank you for your opinion and advice

 

[UWe9o12jkied91d]

Does it mean I don't heat? Don't you think it will take a long time to completely evaporate?
Thank you for your opinion and advice

rezaYes, it's possible, toluene evaporates quite fast even at RT.
You can also heat gently on a water bath

 

[Lev]

Hello, is it possible to order a video synthesis manual? 4-methylpropiophenone

 

[Lev]

Hello William Dampier. Is it possible to buy a video instruction for this synthesis from you?

 

[The-Hive]

I remember when I hive bee done it in 2003 he used


73g aluminium chloride
300mL dichloroethane
46mL propionyl chloride
54mL toluene
600mL iced water
200mL 5% NaOH solution
Magnesium sulfate

 

[Goku]

I remember when I hive bee done it in 2003 he used


73g aluminium chloride
300mL dichloroethane
46mL propionyl chloride
54mL toluene
600mL iced water
200mL 5% NaOH solution
Magnesium sulfate

The-Hiveok but how

 

[The-Hive]

ok but how

GokuIt’s a old one from 2003

 

[Frit Buchner]

I remember when I hive bee done it in 2003 he used


73g aluminium chloride
300mL dichloroethane
46mL propionyl chloride
54mL toluene
600mL iced water
200mL 5% NaOH solution
Magnesium sulfate

The-HiveI couldn't find it either. I searched 4-methylpropriophenone and 5 other names for it

 

[The-Hive]

I couldn't find it either. I searched 4-methylpropriophenone and 5 other names for it

Frit Buchner54mL (500mmol, 46g) toluene was added over 30 minutes to a solution of 73g (550mmol) anhydrous aluminium chloride and 46mL (525mmol, 49g) propionyl chloride in 200ml dichloroethane cooled via an external ice bath. The solution was allowed to stir for a further 1.5 hours at 20oC, and was then carefully added to 500mL stirred iced water. The lower dichloroethane layer was separated off, and the aqueous layer extracted with 2x50mL dichloroethane. The combined extracts were washed with 2x100mL 5% NaOH, 100ml water, and then dried over magnesium sulfate. The solvent was removed, and the ketone vacuum distilled at 123-126oC

 

[Frit Buchner]

dichloroethane. Can't sub it, it's the hydrocarbon backbone(well maybe another halogenated ethane). A fair bit of pain in the ass chems. I hope to go a little more OTC. This could be done by me, the workup is just excessive for where I live (no 190 proof everclear golden -grains. No propoinyl chloride without a license ).

 

[The-Hive]

dichloroethane. Can't sub it, it's the hydrocarbon backbone(well maybe another halogenated ethane). A fair bit of pain in the ass chems. I hope to go a little more OTC. This could be done by me, the workup is just excessive for where I live (no 190 proof everclear golden -grains. No propoinyl chloride without a license ).

Frit BuchnerSee if I got anymore old notes

 

[The-Hive]

dichloroethane. Can't sub it, it's the hydrocarbon backbone(well maybe another halogenated ethane). A fair bit of pain in the ass chems. I hope to go a little more OTC. This could be done by me, the workup is just excessive for where I live (no 190 proof everclear golden -grains. No propoinyl chloride without a license ).

Frit BuchnerWhat I part off the world you in as there’s one with isobutyryl chloride, benzene, aluminum chloride

 

[Frit Buchner]

I've got the one I plan to go with. I certainly don't mind reading some more but.... What I aught to do is build a and go straight from propoinyl chloride I hope to synth and toluene to 4-mp at 105 psi. 7 atmospheres buying chemicals is my cryptonite. Finding references is my superpower. Later, I heard someone was making tartaric acid from cream of tartar and HCl. They can't believe people would buy it
I've came across at least 10 routes to 4 mp

 

[Lev]

 

[Lev]

​

 

[Lev]

 

[The-Hive]

@Frit Buchner how did you get on..​