反应详情

The product from Example 164A (7 g) in 100 mL of THF and tetrabutylammonium fluoride (42 mL of a 1M solution in THF) was heated at reflux for 17 hours, cooled, concentrated to dryness, diluted with 125 mL of ethyl acetate, washed with 5% aqueous NaHCO3, brine, dried over MgSO4, filtered, and the filtrate was concentrated under reduced pressure to provide an oil. The oil was distilled in vacuo (50° C., 1.2 torr) to give 4.9 g of the title compound as a colorless oil.

1. temperatureat reflux for 17 hours
2. temperaturecooled
3. concentrationconcentrated to dryness
4. additiondiluted with 125 mL of ethyl acetate
5. washwashed with 5% aqueous NaHCO3, brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationthe filtrate was concentrated under reduced pressure
9. customto provide an oil
10. distillationThe oil was distilled in vacuo (50° C., 1.2 torr)