Triethylamine → HCID 15163511, compound

Participants

Reaction Steps

A solution of 0.91 g of approximately 85% pure m-chloroperoxybenzoic acid in 20 ml of methylene chloride is added dropwise to a solution of 1.5 g of 2,2-difluoro-6-[(4-methoxy-2-pyridyl)methylthio]-5H-[1,3]-dioxolo[4,5-f]benzimidazole in 50 ml of methylene chloride at -30° C. in the course of 5 min., with stirring, and the temperature is allowed to rise to -10° C. in the course of 30 min. 0.62 ml of triethylamine is added, followed by 20 ml of aqueous potassium bicarbonate solution, the title compound already crystallizing out in the cold. The mixture is filtered and the precipitate is washed with water to yield 1.2 g of the title compound. The organic phase is separated off from the filtrate, washed with water and dried with magnesium sulfate and the solution is concentrated completely, at 30° C. A further 0.25 g of the title compound is obtained from the residue by recrystallization from ethyl acetate; total yield: 92%, m.p.: 184°-185° C. (decompositon).

Provenance & Evidence