反应详情

To a solution of the compound (1.35 g) obtained in Step 7 in phosphorus oxychloride (20 ml) was added water (190 mg) with stirring under ice-cooling, and the mixture was stirred at 100° C. for 3 hr. The reaction mixture was concentrated under reduced pressure, and partitioned by adding chloroform and water. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:10) to give the title compound (1.17 g).

1. temperaturecooling
2. stirringthe mixture was stirred at 100° C. for 3 hr
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. custompartitioned
5. additionby adding chloroform and water
6. washThe organic layer was washed successively with water and saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltrated
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:10)