Coumarins. VI. The Acid-catalyzed Reaction of Phenols with β-Aminocrotononitrile
Kikumasa Sato, Masao Ōhashi, Takeshi Amakasu, K. TAKEDA
Abstract
Kikumasa Sato, Masao Ōhashi, Takeshi Amakasu, K. TAKEDA
Abstract
Abstract A new synthesis of 4-methylcoumarins has been developed by means of the acid-catalyzed condensation of phenols with β-aminocrotononitrile. Such monohydric phenols as phenol or cresols reacted with β-aminocrotononitrile in polyphosphoric acid (PPA) to give 4-methylcoumarins in poor yields, along with a good yield of 6-amino-3-cyano-2,4-lutidine (III). In contrast, 7-substituted-4-methylcoumarins were obtained in 23–44% yields from resorcinol and its monomethyl ether. On the other hand, when β-aminocrotononitrile was heated in PPA, the lutidine (III) was obtained in a high yield. Its precursor, 4-amino-1,3-dicyano-2-methylpenta-1,3-diene (XI), was isolated under mild conditions. These results suggest that β-aminocrotononitrile may undergo the preferential self-dimerization to the lutidine (III) rather than the intermolecular condensation with phenols.
OpenAlex reports 5 citations for this work. Citation counts describe recorded attention and do not establish research quality.
A contribution statement is not available in the OpenAlex record.
Method details are not available in the OpenAlex metadata.
Findings are not separately available in the OpenAlex metadata.
Limitations are not available in the OpenAlex metadata.
Application details are not available in the OpenAlex metadata.
Abstract A new synthesis of 4-methylcoumarins has been developed by means of the acid-catalyzed condensation of phenols with β-aminocrotononitrile. Such monohydric phenols as phenol or cresols reacted with β-aminocrotononitrile in polyphosphoric acid (PPA) to give 4-methylcoumarins in poor yields, along with a good yield of 6-amino-3-cyano-2,4-lutidine (III). In contrast, 7-substituted-4-methylcoumarins were obtained in 23–44% yields from resorcinol and its monomethyl ether. On the other hand, when β-aminocrotononitrile was heated in PPA, the lutidine (III) was obtained in a high yield. Its precursor, 4-amino-1,3-dicyano-2-methylpenta-1,3-diene (XI), was isolated under mild conditions. These results suggest that β-aminocrotononitrile may undergo the preferential self-dimerization to the lutidine (III) rather than the intermolecular condensation with phenols.
Key concepts: Chemistry, Catalysis, Phenols, Organic chemistry, Coumarin