1H-1,2,4-Triazole → 4-Fluoro-3-(fluoromethyl)-3-methyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one

Participants

Reaction Conditions

Reaction Steps

215 g (1 mole) of crude 3,3-bisfluoromethyl-1-bromo-butan-2-one were added dropwise to 84 g (1.2 moles) of 1,2,4-triazole and 165 g (1.2 moles) of ground potassium carbonate in 1 liter of ethanol at 30° to 35° C. The mixture was subsequently stirred at 40° C. overnight, the insoluble material was then filtered off and the filtrate was concentrated. The oily residue was extracted with methylene chloride and water and the extract was dried over sodium sulphate and concentrated. The residue was taken up in methylene chloride and 140 ml of ethereal hydrochloric acid were added. The crystalline product formed was filtered off with suction and extracted by stirring with 1 liter of methylene chloride and 1 liter of saturated aqueous sodium bicarbonate solution, and the extract was washed with 1 liter of water, dried over sodium sulphate and concentrated. 73.8 g (36.4% of theory) of 3,3-bisfluoromethyl-1-(1,2,4-triazol-1-yl)-butan-2-one were obtained as an oil, which could be further reacted directly. ##STR35##

Provenance & Evidence