反应详情

A solution of boron tribromide (1M in DCM, 13.4 mL) was added dropwise to suspension of 2-(2,3-difluoro-4-methoxyphenyl)acetic acid (1.18 g) in DCM (5 mL) at −78° C. The reaction was allowed to warm to RT and stirred overnight. The reaction was cooled to −78° C. and a solution of boron tribromide (1M in DCM, 13.4 mL) was added. The reaction was allowed to warm to RT and stirred for 1 h. The reaction was poured onto ice. The resulting aqueous solution was extracted with DCM (5×50 mL). The aqueous phase was then extracted with ethyl acetate (3×100 mL). The organic solutions were combined, washed with brine (50 mL), dried over magnesium sulphate, filtered and evaporated to give the subtitled compound as a tan solid. Yield 1.09 g.

1. temperatureThe reaction was cooled to −78° C.
2. temperatureto warm to RT
3. stirringstirred for 1 h
4. additionThe reaction was poured onto ice
5. extractionThe resulting aqueous solution was extracted with DCM (5×50 mL)
6. extractionThe aqueous phase was then extracted with ethyl acetate (3×100 mL)
7. washwashed with brine (50 mL)
8. dry with materialdried over magnesium sulphate
9. filtrationfiltered
10. customevaporated