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

Oxygen

Don't buy from me
New Member
Joined
Nov 28, 2021
Messages
1
Reaction score
0
Points
1
There was a alternative for mechanical stirrer?
 

AgamemnonFromTroy

Don't buy from me
Resident
Language
🇺🇸
Joined
Jan 19, 2024
Messages
88
Reaction score
66
Points
18
One 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

Don't buy from me
New Member
Joined
Apr 24, 2022
Messages
3
Reaction score
4
Points
1

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

Moderator in UK section
Resident
Joined
Jun 20, 2023
Messages
496
Reaction score
260
Points
63
Deals
1
I use stainless steel vessel for larger reactions so far so good IMO
 

estimated

Don't buy from me
New Member
Joined
Nov 5, 2022
Messages
2
Reaction score
0
Points
1
hello, can toluene be replaced with xylene?
 

plancklong

Don't buy from me
Resident
Language
🇺🇸
Joined
Jul 7, 2022
Messages
36
Reaction score
13
Points
8
No. The toluene is not just the solvent. It is the basis for the 4-methylpropiophenone:

XFJZp7u8Yi


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

VjTNtYQsw1


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

AgamemnonFromTroy

Don't buy from me
Resident
Language
🇺🇸
Joined
Jan 19, 2024
Messages
88
Reaction score
66
Points
18
You could synthesise toluene from xylene by hydrogenation although toluene is pretty easy to source therefore doing this isn’t that practical.
 
  • Like
Reactions: THR

reza

Don't buy from me
Resident
Joined
Dec 5, 2022
Messages
13
Reaction score
13
Points
3
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

Don't buy from me
Resident
Joined
Aug 8, 2022
Messages
675
Reaction score
510
Points
63
Deals
5
Yes, it's possible, toluene evaporates quite fast even at RT.
You can also heat gently on a water bath
 

Lev

Don't buy from me
Resident
Joined
Mar 14, 2023
Messages
9
Reaction score
9
Points
3
Hello, is it possible to order a video synthesis manual? 4-methylpropiophenone
 

Lev

Don't buy from me
Resident
Joined
Mar 14, 2023
Messages
9
Reaction score
9
Points
3
Hello William Dampier. Is it possible to buy a video instruction for this synthesis from you?
 

The-Hive

Moderator in UK section
Resident
Joined
Jun 20, 2023
Messages
496
Reaction score
260
Points
63
Deals
1
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

Don't buy from me
New Member
Joined
Jul 18, 2023
Messages
23
Reaction score
8
Points
8
ok but how
 

The-Hive

Moderator in UK section
Resident
Joined
Jun 20, 2023
Messages
496
Reaction score
260
Points
63
Deals
1
It’s a old one from 2003
 

Osmosis Vanderwaal

Moderator in US section
Resident
Joined
Jan 15, 2023
Messages
1,600
Solutions
4
Reaction score
1,107
Points
113
Deals
1
I couldn't find it either. I searched 4-methylpropriophenone and 5 other names for it
 

The-Hive

Moderator in UK section
Resident
Joined
Jun 20, 2023
Messages
496
Reaction score
260
Points
63
Deals
1
54mL (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
 

Osmosis Vanderwaal

Moderator in US section
Resident
Joined
Jan 15, 2023
Messages
1,600
Solutions
4
Reaction score
1,107
Points
113
Deals
1
😬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

Moderator in UK section
Resident
Joined
Jun 20, 2023
Messages
496
Reaction score
260
Points
63
Deals
1
See if I got anymore old notes
 

The-Hive

Moderator in UK section
Resident
Joined
Jun 20, 2023
Messages
496
Reaction score
260
Points
63
Deals
1
What I part off the world you in as there’s one with isobutyryl chloride, benzene, aluminum chloride
 

Osmosis Vanderwaal

Moderator in US section
Resident
Joined
Jan 15, 2023
Messages
1,600
Solutions
4
Reaction score
1,107
Points
113
Deals
1
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

Don't buy from me
Resident
Joined
Mar 14, 2023
Messages
9
Reaction score
9
Points
3
:ninja:
 
Last edited:
Top