反应详情

DMF (10 mL) was cooled in an ice bath and phosphorus oxychloride (1.4 mL) added over 20 seconds. The solution was stirred for 10 minutes at room temperature then a solution of the product of step i) (2.0 g) in DMF (4 mL) was added over 5 minutes. The mixture was heated at 95° C. for 16 hours then allowed to cool and poured onto ice/water. The mixture was then extracted into ethyl acetate (100 mL) the organics combined and evaporated under reduced pressure. The residue was purified (SiO2 chromatography, eluting with 1:1 ethyl acetate:isohexane) to give the sub-titled compound (1.5 g).

1. temperatureThe mixture was heated at 95° C. for 16 hours
2. temperatureto cool
3. additionpoured onto ice/water
4. extractionThe mixture was then extracted into ethyl acetate (100 mL) the
5. customevaporated under reduced pressure
6. customThe residue was purified
7. wash(SiO2 chromatography, eluting with 1:1 ethyl acetate:isohexane)