Synthesis of Bisbenzil Isomers and Derivatives.

Abstract

The goal of this investigation was to apply the modified benzoin condensation, used successfully in the synthesis of unsubstituted para-bis(phenylglyoxyloyl) benzene, to the preparation of substituted para-derivatives as well as to the production of selected meta and ortho isomers. Using this process the substituted compounds: p-bis(p-methoxyphenylglyoxyloyl) benzene, p-bis(p-hydroxyphenylglyoxyloyl)benzene, and p-bis(p-chlorophenyl-glyoxyloy) benzene, were obtained yields of 41, 16, and 46%, respectively. The formation of the bis-cyanohydrin intermediate was unequivocally proven by its transformation to the para-bis-hydroxy acid. The extension of the modified benzoin reaction to the synthesis of meta and ortho isomers of p-bis(phenylglyoxyloyl)benzene was to date unsuccessful. In the case of isophthalaldehyde the intermediate bis-cyanohydrin was unexpectedly stable, which under the conditions employed prevented its condensation with benzaldehyde. This material was characterized by the hydrolysis to the meta-bis(hydroxy acid). Reaction of benzaldehyde cyanohydrin with isophthalaldehyde resulted in hydrogen cyanide exchange and formation of the bis-cyanohydrin of isophthalaldehyde and benzaldehyde. The cyanohydrin derived from phthalaldehyde appeared to undergo self-condensation above 0 C; at lower temperatures no reaction with benzaldehyde occurred. (Author)

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Document Details

Document Type
Technical Report
Publication Date
Feb 01, 1976
Accession Number
ADA039083

Entities

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  • Kay L. Paciorek
  • Reinhold H. Kratzer
  • Thomas I. Ito

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  • Counter IED
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  • Acetic Acid
  • Ammonium Nitrate
  • Amorphous Materials
  • Aqueous Solutions
  • Chemical Synthesis
  • Chemistry
  • Corrosion Resistance
  • Glass Transition Temperature
  • Heat Energy
  • Infrared Spectra
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  • Transition Temperature

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  • Chemistry

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  • Organic Chemistry