Home > Community > Synthesis of 2-benzylcyclohexan-1-ol from cyclohexanone
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A Fish in Custard

Synthesis of 2-benzylcyclohexan-1-ol from cyclohexanone

David Petersen  Follow

Making a carbon-carbon bond at the alpha position of a carbonyl suggests using some kind of enolate chemistry. In contrast to an SN2 type reaction with an alkyl halide (which can give over-alkylation and competitive O-alkylation), an aldol condensation is a reliable way to construct the requisite C-C bond. Here cyclohexanone reacted with benzaldehyde under basic conditions gives an enone. Two subsequent reduction steps, hydrogenation followed by hydride addition to the ketone, give the target compound.

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Edward Rosenberg  Follow
However you would probably have to be concerned about dialdol here.More
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Francis B. Banks  Follow
Hmm, wouldnt NaBH4 probably produce the saturated alcohol directly from the α,β-unsaturated carbonyl?More
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James M. Potter  Follow
...or hydrogenate enone over PtO2 or Ni(R) to get double reduction.More
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Fabius Magnus  Follow
@orthocresol You might be right... I thought NaBH4 was pretty selective for the ketone, but quick Google searches support what youre suggesting. Looking thru SciFinder for similar transformations, it looks like more commonly people reduce the ketone first with hydride (NaBH4 or LAH) and then follow up with hydrogenation. Im guessing that hydride will give a mixture of the fully reduced and the allylic alcohol. In practice, youre right. Try NaBH4 first, and if it goes all the way, great. If not, hydrogenation is easy and will finish it off.More
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Frederick Pack  Follow
@Jan Yes, I would... SciFinder had lots of examples of mono-aldol, and theres probably enough of a reactivity difference between cyclohexanone and the mono-aldol product to get good enough selectivity here. Way better than alkylation at least.More
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Dave Obrien  Follow

Mechanism of synthesis

Ok so I found an answer:

  • Deprotonate at the alpha carbon using LDA which gives a negative charge.
  • This then attacks $\ce{BrCH2Ph}$ at the $\ce{CH2}$ and kicks off the bromine in the process ($\mathrm{S_N2}$).
  • Then to form the alcohol the ketone is reduced using $\ce{LiAlH4}$ using THF as a solvent.

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John Murphy  Follow
Alkylation of an enolate is not a reliable reaction. You have to be concerned about over-alkylation and O-alkylation. There are better approaches to this target.More
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Gayantha Vitharanage  Follow
How would one prevent over alkylation? Should I have introduced a protecting group first like a ketal for the carbonyl? How would I protected the other alpha carbon? @jerepierreMore
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Evan McSally  Follow
You can treat cyclohexanone with dimethyl carbonate (THF, NaH) to give the anion of a beta-ketoester. Now alkylate with benzyl bromide followed by aqueous acid hydrolysis and decarboxylation. Extra step but more selective than direct alkylation. One might consider an enamine alkylation.More
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