Water → 2,3-DIFLUORO-6-HYDROXY-5-METHYLBENZALDEHYDE

Participants

Reaction Conditions

Reaction Steps

30 g of 4,5-difluoro-2-methylphenol are dissolved in 180 ml of trifluoroacetic acid and admixed with 57.2 g of hexamethylenetetramine in portions. On completion of addition, the reaction solution is heated to 97-100° C. for 4 hours. After cooling, first 60 ml of 50% sulphuric acid and then 300 ml of water are added dropwise, then the solution is stirred further at room temperature for 2 hours. The reaction solution is extracted three times with methyl tert-butyl ether. The combined extracts are washed once with water and dried, and the solvent is distilled off under reduced pressure. The residue is extracted repeatedly with n-hexane, the extracts are combined and the solvent is distilled off under reduced pressure. 12.5 g (33% of theory) of a bright yellow solid are obtained having a melting point of 53-56° C.

Provenance & Evidence