Sodium Hydroxide → HCID 20253714, compound

Participants

Reaction Steps

A mixture of 8 ml commercially available sodium hypochlorite solution (about 15% of active chlorine) and 5 ml of 10% strength sodium hydroxide solution is added dropwise to a suspension of 1.5 g of 2,2-difluoro-6-[(4-methoxy-5-methyl-2-pyridyl)methylthio]-5H-[1,3-]-dioxolo[4,5-f]benzimidazole in 60 ml of ethyl acetate at 0° C. in the course of 20 min., and stirring is continued at 0° C. for 15 min. 0.5 ml of 10% strength sodium thiosulfate solution and 1.3 g of ammonium sulfate are added, the organic phase is separated off and washed with water, the solution is concentrated in vacuo at 30° C. and the residue is crystallized from ethyl acetate. 1.2 g (74%) of the title compound of m.p. 175°-176° C. (decomposition) are obtained.

Provenance & Evidence