反应详情

温度

25 °C

A solution of the product from Example 107C (22.35 mmol) in toluene (500 mL) was treated with DPPA (5.3 mL, 24.59 mmol) and triethylamine (3.75 mL, 26.90 mmol) was heated at reflux for 2 hours, cooled to 25° C., treated with benzyl alcohol (6.9 mL, 66.68 mmol), heated at reflux for an additional 16 hours, cooled and concentrated. A solution of the concentrate in THF (100 mL) was treated with TBAF solution in THF (67 mL, 1N), stirred at 25° C. for 40 hours, concentrated, and partitioned between ethyl acetate and water. The organic phase was washed with brined, dried over MgSO4, filtered and concentrated, to give the title compound (4.98 g, 37% yield), which was used without further purification.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. temperatureheated
4. temperatureat reflux for an additional 16 hours
5. temperaturecooled
6. concentrationconcentrated
7. concentrationA solution of the concentrate in THF (100 mL)
8. additionwas treated with TBAF solution in THF (67 mL, 1N)
9. concentrationconcentrated
10. custompartitioned between ethyl acetate and water
11. washThe organic phase was washed with brined,
12. dry with materialdried over MgSO4
13. filtrationfiltered
14. concentrationconcentrated