Sciencemadness Discussion Board

Looking for most accessible route to Valerophenone

Jaggermeister - 23-6-2022 at 05:21

Hello,

Ive been looking for a easy accessable route to Valerophenone.

Im in scandinavia, so alot of chemicals are hard to get and most solvents i need to make myself.

One thought is
2-methylbenzaldehyde to its Oxime and then to 2-methylbenzonitrile. But requires many steps and hydroxylamine.

2nd thought is
1-phenylpentan-1-ol or 1-phenylhexan-1-ol and oxidize it to corresponding ketone (Valero or Hexanophenone)

3rd thought is
Pentanoic acid to Pentanoyl chloride by reacting pentanoic acid with thionyl chloride to get Pentanoyl chloride. And then do a FC alkylation of Pentanoyl chloride with Benzene and AlCl3 to get Valerophenone. But thionyl chloride is like impossible to get I assume as its on the chemical weapons list

My goal is to synthesize 2-methyl-PVP, alpha-PVP or alpha-PHP.

I guess oxidation of hexanal or pentanal is a viable route.

Any tips?

[Edited on 23-6-2022 by Jaggermeister]

[Edited on 23-6-2022 by Jaggermeister]

[Edited on 23-6-2022 by Jaggermeister]

Hexabromobenzene - 23-6-2022 at 05:55

Valerophenone can be obtained distillation mixture calcium or magnesium benzoate and valerate
Pentanoic acid can be obtained from sugar

Jaggermeister - 24-6-2022 at 07:30

Quote: Originally posted by Hexabromobenzene  
Valerophenone can be obtained distillation mixture calcium or magnesium benzoate and valerate
Pentanoic acid can be obtained from sugar

Ive heard that dry distillation of calcium benzoate and Valerate produce Valerophenone, but i cant find a single reputable source for this claim.

arkoma - 24-6-2022 at 07:43

Jaggermeister, please first be welcome, second please carefully read site rules. No blatant spoon-feeding for illegal drug manufacturer is tolerated here. Even on a drug chem oriented site you would get called on such a spoon-feed.

Please do a bit more delving on your own and UTFSE (Use the*uckingSearchEngine) please.

Thank you, Arkoma

Edit-forum FAQ, Sorry
Quote:

Do not request spoonfeeding of information for clandestine drug manufacture. However, every sort of chemistry is a permissible topic of discussion if you discuss it like a scientist.


If you read some of the threads that seem in violation of this you will find that they are actual experimental procedures performed by members, and written up in a clear and scientific (organized at least) manner. Not spoon-feeding. Again, welcome aboard, and learn the pleasures of being an autodidact!

[Edited on 6-24-2022 by arkoma]

[Edited on 6-24-2022 by arkoma]

Jaggermeister - 24-6-2022 at 08:44

Quote: Originally posted by arkoma  
Jaggermeister, please first be welcome, second please carefully read site rules. No blatant spoon-feeding for illegal drug manufacturer is tolerated here. Even on a drug chem oriented site you would get called on such a spoon-feed.

Please do a bit more delving on your own and UTFSE (Use the*uckingSearchEngine) please.

Thank you, Arkoma

Edit-forum FAQ, Sorry

Quote:

Do not request spoonfeeding of information for clandestine drug manufacture. However, every sort of chemistry is a permissible topic of discussion if you discuss it like a scientist.


If you read some of the threads that seem in violation of this you will find that they are actual experimental procedures performed by members, and written up in a clear and scientific (organized at least) manner. Not spoon-feeding. Again, welcome aboard, and learn the pleasures of being an autodidact!

[Edited on 6-24-2022 by arkoma]

[Edited on 6-24-2022 by arkoma]

I have ben researching different routes for a year. I would definately not call this spoon feeding. Looking om pointers of most accessible route of The routes ive researched is not asking to be spoonfed.

If u think it is, Then we must agree to disagree and you May leave The thread. I tried my best not to sound condescendinf. If u find i did anyway, then I apologise.

DocX - 25-6-2022 at 10:59

I think Aroma is trying to do you a favour. Spoonfeeding or not aside, from what I've seen, threads with these kind of themes are tolerated better if they're done like prepublication posts, with pictures of performed syntheses and complete lists of citations, trials and tribulations.

Just a tip. Check out the threads by user Benignium, they're the perfect examples.
And good luck with your quest, sorry if I can't help you with the actual synthesis. I'd love to see whatever you try out though!

[Edited on 20222222/6/25 by DocX]

Mush - 25-6-2022 at 13:12

Quote: Originally posted by Hexabromobenzene  
Valerophenone can be obtained distillation mixture calcium or magnesium benzoate and valerate Pentanoic acid can be obtained from sugar


Mailhe
Comptes Rendus Hebdomadaires des Seances de l'Academie des Sciences, 1913, vol. 157, p. 221
Bulletin de la Societe Chimique de France, 1914, vol. ,4, 15, p. 325



FC alkylation of Pentanoyl chloride with Benzene

Layraud
Bulletin de la Societe Chimique de France, 1906, vol. 3, 35, p. 233

karlos³ - 25-6-2022 at 14:06

Grignard, butylmagnesium halide and benzaldehyde, gives "fenipentol", 1-phenylpentan-1-ol.
Since you are going to brominate and consequently substitute that part with an amine, you could simply do the oxidation/bromination/amination one-pot with NBS?

Reference for all three reactions one-pot: https://doi.org/10.1002/slct.201803465
If you look into that direction further, you will find reactions like that which are not making use of DBU as organic base, possibly something much more accessible, and directly with an amination using pyrrolidine instead of an imidation with succinimide.

draculic acid69 - 28-6-2022 at 00:31

Quote: Originally posted by Hexabromobenzene  
Valerophenone can be obtained distillation mixture calcium or magnesium benzoate and valerate
Pentanoic acid can be obtained from sugar


Can you please provide link to post or refs on the sugar to pentanoic acid

[Edited on 28-6-2022 by draculic acid69]