反应详情

A solution of 2.98 g (13.3 mmol) of the compound from Example 48A in toluene (25.0 ml) was admixed under argon at RT with 3.62 g (16.7 mmol) of the compound from Example 33A in ethanol (8.4 ml) and 2.03 g (14.7 mmol) of potassium carbonate. After stirring for 10 min, 1.54 g (1.34 mmol) of tetrakis(triphenylphosphine)palladium and then 2.33 g (40.0 mmol) of potassium fluoride in water (5.8 ml) were added. The mixture was stirred under reflux for 8 h, and the reaction solution was cooled and diluted with ethyl acetate. The reaction solution was washed in water, and the organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue was purified by means of column chromatography (silica gel, dichloromethane/methanol 100:1→80:1). Yield: 2.62 g (69% of theory, 4:1 mixture of methyl and ethyl ester)

1. stirringThe mixture was stirred
2. temperatureunder reflux for 8 h
3. temperaturethe reaction solution was cooled
4. washThe reaction solution was washed in water
5. dry with materialthe organic phase was dried over magnesium sulphate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by means of column chromatography (silica gel, dichloromethane/methanol 100:1→80:1)
9. additionYield: 2.62 g (69% of theory, 4:1 mixture of methyl and ethyl ester)