反应详情

A solution of the product from step (vii) (9.5 g) in thionyl chloride (100 ml) was stirred at room temperature for 4 days. After removal of solvent under reduced pressure, the residue was dissolved in 1,2-dichloroethane (200 ml) and treated with aluminium chloride (23 g). The reaction mixture was heated at reflux for 1 hour and allowed to cool. The resultant suspension was partitioned between 10% hydrochloric acid and dichloromethane. The combined extracts were evaporated, triturated with acetonitrile, and filtered through a plug of celite. Evaporation afforded a residue which was purified by chromatography eluting with 50-100% ethyl acetate in isohexane.

1. customAfter removal of solvent under reduced pressure
2. dissolutionthe residue was dissolved in 1,2-dichloroethane (200 ml)
3. additiontreated with aluminium chloride (23 g)
4. temperatureThe reaction mixture was heated
5. temperatureat reflux for 1 hour
6. temperatureto cool
7. customThe resultant suspension was partitioned between 10% hydrochloric acid and dichloromethane
8. customThe combined extracts were evaporated
9. customtriturated with acetonitrile
10. filtrationfiltered through a plug of celite
11. customEvaporation
12. customafforded a residue which
13. customwas purified by chromatography
14. washeluting with 50-100% ethyl acetate in isohexane