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Alan Armstrong

Effect of Zn dust reduction of phenolic -OH group on other groups

Amos Ekeson  Follow

I did some research for this question many years ago. Nisarg's answer prompted me to post an answer.


Nisarg's answer showed how nitrobenzene can be reduced to form different compounds but my answer focuses on some different compounds. Doing some literature surveys gave me results from very old books. All the reaction involves only zinc dust. I tried quoting but the majority of the terms/compound names are obsolete, so I have wrote them as points:

  • formanilide and its derivatives is reduced benzenenitrile and aniline (and its derivatives) as major products and other side products such as N-Methyldiphenylamine. Yield of nitrile 10-20% weight of initial formanilide.
  • N-alkyl-o-toluidine and N-alkyl-p-toluidine yields corresponding nitrile: yield 15-20%
  • methyl-α- and methyl-β-naphthalamine yield α- and β-naphthonitrile
  • xylidine and its isomers yields xylonitrile (prone to hydrolysis to yield xylic acid(isomeric carboxylic acid of xylene)) : yield 12%
  • Phenyl isothiocyanate and thiocarboanilide forms benzonitrile and some aniline.

References:

  1. K.Gasiorowski and V.Merz, Journal of the Chemical Society, 1884

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James Sampley  Follow
Do these reactions occur in pure zinc dust distillation or do they require NaOH, NH4Cl etc.?More
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Haider Ali  Follow
@SRMaiti only zinc dust is used. No other catalyst/reagent used.More
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Ayesha Khan  Follow

Out of the groups you mention $\ce{-NO2}$, $\ce{-CN}$ will most certainly react, $\ce{-CH3}$ and $\ce{-NH2}$ not so much and I am ambiguous about $\ce{-CONH2}$.

Although I said that $\ce{-CN}$ will react, I can't pin point the product which will form in a certain condition. But in case of $\ce{-NO2}$, I certainly can predict the product based on a list I complied a couple of years ago.

The "List":

$$\begin{array}{|ccc|}\hline\ce{Ph-NO2}&\xrightarrow[\ce{NH4Cl}]{\ce{Zn}}&\ce{Ph-NHOH}\\\hline\ce{Ph-NO2}&\xrightarrow[\ce{NaOH}]{\ce{Zn}}&\ce{Ph-NH-NH-Ph}\\\hline\ce{Ph-NO2}&\xrightarrow[\ce{NaOH}]{\ce{Zn+alcohol}}&\ce{Ph-N=N-Ph}\\\hline\end{array}$$


References:

(1) Kamm, O. β-Phenylhydroxylamine". Organic Syntheses. ; Collective 1941, 1, 445.

(2) Bigelow, H. E.; Robinson, D. B. Azobenzene". Organic Syntheses. ; Collective 1955, 3, 103.

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Geoffrey Roberts  Follow
. This reaction is somewhat similar to More
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Eric Johnson  Follow
cyanobenzene does react with zinc dust and bromoacetic acid to form a red crystalline compoundMore
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Jeremy Kennedy  Follow
Why doesalcohol cause it to become double bondMore
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Geraldine Merola  Follow
@Buraian Possibly condensation. My guess: The reaction creates nitroso and hydroxylamine products which then condense to azoxy and then ultimately to azo product.More
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H?kon Hapnes Strand  Follow
@Nisarg As a side note: Although this doesnt count as reduction but More
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