反应详情

温度

90 °C

A solution/suspension of compound 59 (0.184 g, 0.44 mmol) in toluene was treated with phosphorus oxychloride (1 ml) and stirred at 90° C. under a nitrogen atmosphere for 22.5 h. The mixture was cooled and treated with water (20 ml) then neutralised by addition of solid sodium hydrogen carbonate. The mixture was then extracted with ethyl acetate (2×25 ml) and the organics separated and dried over sodium sulphate, filtered and evaporated to dryness. The residue was chromatographed on silica gel eluting with an ethyl acetate/isohexane gradient to give the title compound as a yellow oil (0.092 g, 52%).

1. temperatureThe mixture was cooled
2. extractionThe mixture was then extracted with ethyl acetate (2×25 ml)
3. customthe organics separated
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated to dryness
7. customThe residue was chromatographed on silica gel eluting with an ethyl acetate/isohexane gradient