反应详情

温度

50 °C

In a solution of 1-(2,4-dihydroxyphenyl)-2-(4-hydroxyphenyl)-ethanone (2 mmol) in DMF (6 mL), freshly distilled BF3.OEt2 (6.3 mL) was added under argon. The mixture was heated at 50° C., and a solution of methanesulphonyl chloride (1 mL) in dry DMF (1.5 mL) was added slowly. After reaction at 80° C. for 1 h, the mixture was cooled to rt and poured into a large volume of ice cold aq. sodium acetate (12 g/100 mL), then extracted with EtOAc, and the organic layer was dried and concentrated. The residue was purified by column chromatography on silica gel using a mixture of DCM and MeOH to give 7-hydroxy-3-(4-hydroxyphenyl)-chromen-4-one.

1. customAfter reaction at 80° C. for 1 h
2. temperaturethe mixture was cooled to rt
3. extractionextracted with EtOAc
4. customthe organic layer was dried
5. concentrationconcentrated
6. customThe residue was purified by column chromatography on silica gel using
7. additiona mixture of DCM and MeOH