反应详情

温度

25 °C

A solution containing the product from Example 107B (10.55 g, 22.35 mmol) in a mixture of dioxane (130 mL) and water (65 mL) was treated with sodium hydroxide solution (33.5 mL, 1N), stirred for 30 minutes at 25° C., concentrated, cooled to 0° C., acidified to pH 5 using 10% citric acid, and partitioned between dichloromethane and water. The organic phase layer was washed with brine, dried over Na2SO4, filtered and concentrated. A solution of the concentrate in dimethylformamide (130 mL) was treated with imidazole (18.3 g, 268.80 mmol) and t-butyldimethylsilyl chloride (20.2 g, 134.01 mmol), stirred at 25° C. for 16 hours, and concentrated. The concentrate was combined with ice and extracted with ethyl acetate. The organic phase was washed with 10% citric acid and brine, dried over MgSO4, filtered, and concentrated. A solution of the residue in a mixture of THF (100 mL), acetic acid (100 mL) and water (33 mL) was stirred at 25° C. for 2 hours, and concentrated under reduced pressure. The residue was dissolved in toluene and concentrated several times, followed by drying under high vacuum to give the title compound, which was used without further purification.

1. concentrationconcentrated
2. temperaturecooled to 0° C.
3. custompartitioned between dichloromethane and water
4. washThe organic phase layer was washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. concentrationA solution of the concentrate in dimethylformamide (130 mL)
9. stirringstirred at 25° C. for 16 hours
10. concentrationconcentrated
11. extractionextracted with ethyl acetate
12. washThe organic phase was washed with 10% citric acid and brine
13. dry with materialdried over MgSO4
14. filtrationfiltered
15. concentrationconcentrated
16. additionA solution of the residue in a mixture of THF (100 mL), acetic acid (100 mL) and water (33 mL)
17. stirringwas stirred at 25° C. for 2 hours
18. concentrationconcentrated under reduced pressure
19. dissolutionThe residue was dissolved in toluene
20. concentrationconcentrated several times
21. customby drying under high vacuum