반응 #648789

ord-09735d6cf1794adb9161991344aef5df

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the phases were separated
  2. 2
    추출The aqueous phase was extracted with dichloromethane
  3. 3
    세척The combined organic phases were washed with saturated aqueous sodium chloride solution
  4. 4
    건조dried over sodium sulfate
  5. 5
    여과filtered
  6. 6
    농축concentrated
  7. 7
    기타The residue was purified by preparative HPLC (mobile phase: acetonitrile/water gradient)

실험 절차

A solution of 740 mg (1.84 mmol) of the compound from Example 104A in 20 ml of tetrahydrofuran was added dropwise to 5.5 ml (5.5 mmol) of a 1N solution of diisobutylaluminum hydride in dichloromethane in 20 ml of tetrahydrofuran at RT under argon. The mixture was stirred at RT for 2 h and then water and dichloromethane were added, and the phases were separated. The aqueous phase was extracted with dichloromethane. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The residue was purified by preparative HPLC (mobile phase: acetonitrile/water gradient). 437 mg (66% of theory) of the title compound were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08063234B2uspto-grants-2011_11