Methanesulfonyl chloride → HCID 76710727, compound

Participants

Reaction Conditions

Reaction Steps

To an ice-cooled and stirred solution of ethyl 2-({2-hydroxy-4-[4-(methylsulfonyl)phenoxy]phenyl}hydrazono)propanoate (5.8 g) in pyridine (60 mL) was added methanesulfonyl chloride (1.4 mL), and the mixture was stirred at 4° C. for 1 h and then at room temperature for 3 h. The reaction mixture was concentrated in vacuo and the residue was partitioned between ethyl acetate and aqueous citric acid solution. The organic layer was washed successively with aqueous citric acid solution and brine, dried (MgSO4), filtered, and concentrated in vacuo. The residue was purified by short silica gel chromatography (ethyl acetate) to give light orange crystals, which were washed with ethyl acetate-hexane to give the title compound (6.49 g, 93%) as light orange crystals. MS 471 (MH+).

Provenance & Evidence