反応 #50106

ord-a254a47f4a7b42b890ab20256a72c77c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to return to room temperature
  2. 2
    その他(1 h 30 min)
  3. 3
    抽出the mixture was extracted with dichloromethane (4×10 cm3)
  4. 4
    乾燥The extract was dried over MgSO4
  5. 5
    ろ過filtered
  6. 6
    その他evaporated down
  7. 7
    その他The crude product was purified by flash chromatography on silica (eluent ether/petroleum ether=5/95)

実験手順

2.91 cm3 (2.91 mmol) of BBr3 in molar solution in dichloromethane were introduced at 4° C. under argon atmosphere into 0.98 (5.3 mmol) of epoxide 2e in solution in 6.5 cm3 dichloromethane. The reaction mixture was then allowed to return to room temperature and stirring was continued (1 h 30 min). 5 cm3 of distilled water were then added and the mixture was extracted with dichloromethane (4×10 cm3). The extract was dried over MgSO4, filtered and evaporated down. The crude product was purified by flash chromatography on silica (eluent ether/petroleum ether=5/95): 1.03 g of alcohol 1i were obtained (macrobore GC purity>97%); the yield of product 1i was 73%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05424460uspto-grants-1995_06