3-Hydroxybenzoic Acid → HCID 21413335, compound

Participants

Reaction Steps

178 parts of 45% strength sodium hydroxide solution are added dropwise to a suspension of 460 parts of 93% strength 4,6-dichloro-2-aminophenol hydrochloride in 1,500 parts by volume of dichlorobenzene mixture at 110° to 120°, under a nitrogen atmosphere, 30 parts of boric acid and 276 parts of 3-hydroxy-benzoic acid are added to the resulting clear solution and the water is removed from the system by means of a water separator (about 10 hours). The hot reaction solution is then poured into about 2,500 parts by volume of n-butanol, the hot solution is clarified with fuller's earth and after cooling and, if necessary, further concentrating, about 280 to 290 parts of 2-(3'-hydroxyphenyl) 5,7-dichlorobenzoxazole are obtained, which can be purified further by recrystallisation from chlorobenzene (melting point 233° to 234°). Molecular weight, calculated and confirmed by mass spectrometry at m/e = 280.

Provenance & Evidence