反应详情

LiBr (1.03 g) is added to a solution of NaBH4 (0.45 g) in THF (15 ml). The reaction mixture is heated at reflux for 7 hours, and the compound obtained in Step B (1.3 g) is added, followed by B(OMe)3 (0.067 ml). After refluxing for 18 hours, the mixture is concentrated under reduced pressure and the residue obtained is taken up in 20 ml of 3N H2SO4. The aqueous phase is saturated with NaCl and extracted with ethyl acetate. The organic phase is dried over magnesium sulphate, filtered and evaporated to dryness. The residue is purified on silica gel (SiO2, eluant: AcOEt) to yield the title product in the form of a beige solid. The compound obtained is used directly in the next reaction.

1. temperatureThe reaction mixture is heated
2. temperatureat reflux for 7 hours
3. temperatureAfter refluxing for 18 hours
4. concentrationthe mixture is concentrated under reduced pressure
5. customthe residue obtained
6. extractionextracted with ethyl acetate
7. dry with materialThe organic phase is dried over magnesium sulphate
8. filtrationfiltered
9. customevaporated to dryness
10. customThe residue is purified on silica gel (SiO2, eluant: AcOEt)