Acetic Anhydride → HCID 15096587, compound

Participants

Reaction Steps

Five (5) g (0.0141 mol) of 4,4,4-trichloro-2-(4-chlorophenyl)-2-hydroxy-(1,2,4-(1H)-triazolyl)butane (prepared as in Example I) was slurried in 75 mls of benzene, 4.31 g (0.0422 mol) of acetic anhydride and 2.6 g (0.0211 mol) of 4-dimethylaminopyridine. This mixture was stirred at room temperature for 30 hours and then diluted with 75 mls of benzene. The mixture was washed thrice with 100 mL portions of water. Evaporation of the solvent under reduced pressure and purification of the residue by preparative high pressure liquid chromatography (HPLC) in a 1:1 mixture of ethyl acetate and hexane gave the desired product as a white solid in a yield of 2.2 g (39 percent of theoretical) melting at 112°-114° C.

Provenance & Evidence