Water → HCID 73796237, compound

Participants

Reaction Steps

A mixture of 1-difluoromethylthio-3,3-dimethyl-2-butanone (2.21 moles) from example 1, hydroxylamine hydrochloride (2.44 moles) and sodium carbonate (1.22 moles) in aqueous ethanol (1 liter of water and 2.3 liters of ethanol) was heated at its reflux temperature for 7.5 hours. This reaction mixture was poured into water, and the product was extracted into diethyl ether. The ether was washed with water and dried, then the ether extracts were evaporated under reduced pressure leaving a residue of 1-difluoromethylthio-3,3-dimethyl-2-butanone oxime. A pure sample, m.p. 92° to 95°C., was obtained by recrystallization from a mixture of diethyl ether and petroleum ether (b.p. 30° to 60°C.).

Provenance & Evidence