반응 #72583
ord-5cacf02494ab456aa5d2a63bfab4ce5b
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The reaction mixture is heated
- 2온도at reflux for 7 hours
- 3온도After refluxing for 18 hours
- 4농축the mixture is concentrated under reduced pressure
- 5기타the residue obtained
- 6추출extracted with ethyl acetate
- 7건조The organic phase is dried over magnesium sulphate
- 8여과filtered
- 9기타evaporated to dryness
- 10기타The residue is purified on silica gel (SiO2, eluant: AcOEt)
실험 절차
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.