反应详情

To a slurry of the product of step (iii) (1.1 g) in dry 1,2-dichloroethane (20 ml) was added bis(trimethylsilyl)trifluoroacetamide (1.9 ml) under nitrogen. The mixture was heated under reflux for 1 hour until the mixture became a homogeneous solution. The solution was allowed to cool to room temperature and a solution of the product of step (ii) (0.83 g) in dry acetonitrile (10 ml) was added. The solution was then heated at reflux for 7 hours. The reaction mixture was allowed to cool and evaporated under reduced pressure. Purification was by chromatography eluting with 30% ethyl acetate in toluene. The resulting oil was triturated with diethyl ether/isohexane to give the product as a cream solid. Yield 1.52 g.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 1 hour until the mixture
3. temperatureThe solution was then heated
4. temperatureat reflux for 7 hours
5. temperatureto cool
6. customevaporated under reduced pressure
7. customPurification
8. washeluting with 30% ethyl acetate in toluene
9. customThe resulting oil was triturated with diethyl ether/isohexane