反应详情

温度

70 °C

To a stirring solution of 3,4-dimethoxy-2-(methoxymethyl)phenylboronic acid (Compound 301) (3.5 g, 16.58 mmol) in dimethylformamide (50 mL) under nitrogen atmosphere, were added cesium carbonate (16.17 g, 49.75 mmol), tetrakis(triphenylphosphine) palladium(0) (957 mg, 0.828 mmol) and 5-bromoisobenzofuran-1(3H)-one (8.02 g, 33.14 mmol) and the resultant reaction mixture was heated to 70° C. for 3 h. The reaction mixture was filtered off and the filtrate was extracted with ethyl acetate (3×). The combined ethyl acetate layer was washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. Purification by column chromatography (silica gel, 0-30% ethyl acetate in pet ether) afforded 5-(3,4-dimethoxy-2-(methoxymethoxy)phenyl)isobenzofuran-1(3H)-one as a solid.

1. customthe resultant reaction mixture
2. filtrationThe reaction mixture was filtered off
3. extractionthe filtrate was extracted with ethyl acetate (3×)
4. washThe combined ethyl acetate layer was washed with brine
5. dry with materialdried over anhydrous sodium sulphate
6. concentrationconcentrated under reduced pressure
7. customPurification by column chromatography (silica gel, 0-30% ethyl acetate in pet ether)