반응 #74501

ord-3270066dc9494738a1fed70eb9f13b4f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with EtOAc
  2. 2
    세척The organic layer was washed with water
  3. 3
    건조brine, dried over anhydrous MgSO4
  4. 4
    여과filtered
  5. 5
    농축concentrated in vacuo
  6. 6
    기타The crude residue was purified by column chromatography (3-10% EtOAc/hexanes)

실험 절차

To a solution of (3-bromonaphthalen-1-yl)methanol in DMF (100 mL) was added imidazole (6.4 g, 93 mmol), DMAP (0.57 g, 4.7 mmol), and TIPSCl (15 mL, 70 mmol). The resulting solution was stirred at room temperature for 12 h, diluted with a saturated ammonium chloride and extracted with EtOAc. The organic layer was washed with water then brine, dried over anhydrous MgSO4, filtered and concentrated in vacuo. The crude residue was purified by column chromatography (3-10% EtOAc/hexanes) to yield the title compound (17.9 g, 96%) as a colorless oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541380B2uspto-grants-2013_09