Boron tribromide → HCID 23062636, compound

Participants

Reaction Steps

To the suspension of (2-cyano-4-methoxyphenoxy)-N-(5-chloropyridin-2-yl)acetamide (40.0 g) obtained in Reference Example 59 in dichloromethane (2000 ml), boron tribromide (173 g) is added at −58° C. dropwise over 40 minutes. The reaction solution is stirred for 26 hours with keeping the internal temperature between −20° C. and 0° C., and then poured to an ice-water. The precipitated solid is collected by filtration, washed with water, and then dried under reduced pressure. A part of the resulting solid (37.2 g), i.e. 24.3 g thereof is purified by silica gel column chromatography (eluent: chloroform/methanol=50/1-10/1) to give the title compound (17.0 g).

Provenance & Evidence