反应详情

A mixture of palladium acetate (0.045 g) and tri-p-tolylphosphine (0.213 g) in methanol (10 ml) was stirred at RT for 30 min. The product from step (iii) (1 g), sodium carbonate (1.27 g), the product from example (26) step (i) (1.19 g) and methanol (20 ml) were added and the mixture heated under reflux for 6 h. The solvent was removed under reduced pressure and the residue partitioned between diethylether and 2M hydrochloric acid. The organics were separated, dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with 10% ethylacetate/isohexane. Yield 0.503 g

1. temperaturethe mixture heated
2. temperatureunder reflux for 6 h
3. customThe solvent was removed under reduced pressure
4. customthe residue partitioned between diethylether and 2M hydrochloric acid
5. customThe organics were separated
6. customdried
7. customevaporated under reduced pressure
8. customThe residue was purified by chromatography on silica eluting with 10% ethylacetate/isohexane