4-Chloro-2-nitrobenzoic acid → HCID 67050100, compound

Participants

Reaction Steps

To a solution of 4,5-difluoro-benzene-1,2-diamine (2.0 g, 6.94 mmol; CAS Reg. No. 76179-40-3) in o-xylene (25 ml) was added 4-chloro-2-nitro-benzoic acid (2.78 g, 6.94 mmol; CAS Reg. No. 6280-88-2) and titanium tetraethoxide (2.9 ml, 6.94 mmol) at 25° C., and the reaction mixture was allowed to stir at reflux temperature for 14 h. After the completion of reaction, solvents were evaporated under reduced pressure. The residue was purified by column chromatography over silica gel (18-20% ethyl acetate/n-hexane) to afford the desired compound as a yellow powder (15%). MS (Turbo Spray): m/z=310.2 (M+H).

Provenance & Evidence