Ammonia → HCID 178429547, compound

Participants

Reaction Conditions

Reaction Steps

3-cyano-4-methyl-6-hydroxypyrid-2-one is prepared by running 99 parts of cyanoacetic acid methyl ester into 160 parts of 24% strength aqueous ammonia, while stirring, at 10° to 15° C. The mixture is stirred for approx. 1 hour at 20° C., 133.5 parts of acetoacetic acid methyl ester are then added and the reaction mixture is heated at 80° C. for 4 hours in an autoclave, a maximum pressure of 1.5 bars being generated. The reaction suspension is then diluted with 400 parts of water and 114 parts of 61% strength sulphuric acid are added at 50°-60° C. and the mixture is cooled to 20° C. The product precipitated is filtered off, washed with water and dried. This gives 147.0 parts (98% of theory) of 3-cyano-4-methyl-6-hydroxypyrid-2-one with a melting point above 305° C.

Provenance & Evidence