反应详情

Thionyl chloride (180 ml) was added to the product of step (iii) (45.5 g) at 0° C. The mixture was stirred at room temperature for 2 hours and heated at reflux for 40 min. The residue after evaporation under reduced pressure was dissolved in ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase was dried (MgSO4) and solvent evaporated under reduced pressure. Purification was by chromatography eluting with 1-2% ethanol in dichloromethane to give the subtitle product as an orange oil.

1. temperatureheated
2. temperatureat reflux for 40 min
3. customThe residue after evaporation under reduced pressure
4. dissolutionwas dissolved in ethyl acetate
5. washwashed with saturated sodium bicarbonate solution
6. dry with materialThe organic phase was dried (MgSO4) and solvent
7. customevaporated under reduced pressure
8. customPurification
9. washeluting with 1-2% ethanol in dichloromethane