反应详情

A solution of 6.78 g (23.7 mmol, purity 90%) of the compound from Example 74A in toluene (339 ml) was admixed under argon at RT with 7.74 g (35.6 mmol) of the compound from Example 29A in ethanol (112 ml) and 3.61 g (26.1 mmol) of potassium carbonate. After stirring for 10 min, 2.74 g (2.37 mmol) of tetrakis(triphenylphosphine)palladium and then 4.14 g (71.2 mmol) of potassium fluoride in water (71 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, dichloromethane/methanol 150:1→100:1). The product fractions were concentrated under reduced pressure and the solid obtained was purified by stirring with diethyl ether. Yield: 6.00 g (50% of theory, purity 62%)

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, dichloromethane/methanol 150:1→100:1)
9. concentrationThe product fractions were concentrated under reduced pressure
10. customthe solid obtained
11. customwas purified
12. stirringby stirring with diethyl ether