반응 #304950

ord-7df822b9d62d4de1af2f7511b62d0731

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출The reaction mixture was extracted with dichloromethane
  2. 2
    세척washed with water (×3)
  3. 3
    건조The combined organic layer was dried over anhydrous MgSO4
  4. 4
    여과filtered
  5. 5
    농축concentrated in vacuo
  6. 6
    기타The crude product was purified by column chromatography with PE

실험 절차

To a solution of the product of step (i) (32.25 g, 0.15 mol) in anhydrous dichloromethane (400 mL) was added triethylamine (45 g, 0.45 mol), DMAP (915 mg, 7.5 mmol) and TBSCl (33 g, 0.215 mol) sequentially. The resulting solution was stirred overnight. The reaction mixture was extracted with dichloromethane and washed with water (×3). The combined organic layer was dried over anhydrous MgSO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography with PE to afford the subtitle compound (ii) as a pale brown oil (40 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08198285B2uspto-grants-2012_06