Water → HCID 13019448, compound

Participants

Reaction Conditions

Reaction Steps

17.3 g (0.05 mol) of 1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-1-(imidazol-1-yl)-butan-2-ol were dissolved in 100 ml of acetic anhydride and, after adding 0.1 g of sodium acetate, the mixture was stirred at 100° C. for 10 hours. Thereafter, the reaction solution was allowed to cooled to room temperature, stirred into 500 ml of water and left to stand for 15 hours. The aqueous phase was extracted twice with 200 ml of methylene chloride each time. The combined organic phases were washed with 100 ml each of sodium bicarbonate solution and water, dried over sodium sulphate and concentrated in vacuo. The residue was taken up in 100 ml of ether, 20 ml of ethereal hydrochloric acid were added, the solvent was distilled off in vacuo and the residue was stirred with 50 ml of ether. 15.3 g (72% of theory) of 2-acetoxy-1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-1-(imidazol-1-yl)-butane hydrochloride of melting point of 198°-200° C. were obtained.

Provenance & Evidence