反应详情

温度

0 °C

Boron tribromide (393 μl, 4.16 mmol) was added dropwise to a solution of ethyl[4-({[6-chloro-2-fluoro-3-(methyloxy)phenyl]carbonyl}amino)phenyl]acetate (506 mg, 1.39 mmol) in dichloromethane (30 ml) at −78° C. under argon and the reaction was stirred overnight whilst slowly warming to 0° C. The reaction was quenched by the careful addition of water, stirred for 1 hour, further diluted with ethyl acetate, filtered, phases separated, the organic layer dried (Na2SO4) and solvent evaporated and the residue purified by flash chromatography (Biotage SP4, 25+M silica column, 0→80% ethyl acetate/petrol, clean fractions collected) to afford the title compound as a colourless foam (157 mg, 32%).

1. customThe reaction was quenched by the careful addition of water
2. stirringstirred for 1 hour
3. additionfurther diluted with ethyl acetate
4. filtrationfiltered
5. customphases separated
6. dry with materialthe organic layer dried (Na2SO4) and solvent
7. customevaporated
8. customthe residue purified by flash chromatography (Biotage SP4, 25+M silica column, 0→80% ethyl acetate/petrol, clean fractions collected)