Phosphorus oxychloride → HCID 18760214, compound

Participants

Reaction Steps

A mixture of 6-chloro-2-[(4-fluorophenyl)amino]-3-nitrobenzoic acid (12.39 g, 0.04 mol), chloroform (100 ml), and POCl3 (60 ml, 0.64 mol) was stirred at reflux for 8 h. Solvents were removed under reduced pressure. To the residue was added 200 ml of a mixture of 1,4-dioxane and water (8:1), and the mixture was acidified with concentrated hydrochloric acid and stirred at reflux for 2 h. Water was added (200 ml) and the precipitate was collected by filtration and crystallized from N,N-dimethylformamide—water to give 10.2 g (87%) of 1b as orange needles: mp 287-291° C. Anal. (C13H6N2O3ClF) C, H, N.

Provenance & Evidence