반응 #49175

ord-d8e7cc59633842469a6293c295a59251

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타evaporated dryness
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane (300 mL)
  3. 3
    세척It was washed with saturated NaHCO3 aqueous solution (3×100 mL)
  4. 4
    건조The organic layer was dried over Na2SO4
  5. 5
    여과filtered
  6. 6
    기타evaporated to dryness

실험 절차

Compound 17 (10.5 g, 22 mmol) was dissolved in anhydrous dichloromethane (150 mL). To the solution were added disuccinimidyl carbonate (8.45 g, 33 mmol), triethylamine (20 mL) and acetonitrile (50 mL). The reaction mixture was stirred at room temperature under argon for over night and then evaporated dryness. The residue was dissolved in dichloromethane (300 mL). It was washed with saturated NaHCO3 aqueous solution (3×100 mL). The organic layer was dried over Na2SO4, filtered and evaporated to dryness. Compound 18 (10.4 g, 77%) was obtained as colorless powder after drying in high vacuum, which was directly used for the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745608B2uspto-grants-2010_06