반응 #47714

ord-99507a7d432941919231c95eaa923a8e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated
  2. 2
    workup.ADDITIONThe residue was diluted with 50 mL of methylene chloride
  3. 3
    농축concentrated via rotary evaporation
  4. 4
    workup.ADDITIONThe residue was then diluted with 50 mL of methanol
  5. 5
    농축re-concentrated via rotary evaporation
  6. 6
    workup.ADDITIONThe residue was again re-diluted with 50 mL of methylene chloride
  7. 7
    농축re-concentrated, first via rotary evaporation

실험 절차

To a 250 mL round bottom flask, charged with 1.50 g (1.75 mmol) of N—BOC—N,N-bis-(N′,N′-bis(5-methoxycarbonylpentyl)-5-carbamyl pentyl)-amine (17) in 15 mL of methylene chloride, was added 15 mL of trifluoroacetic acid. The mixture was stirred at room temperature for 15 minutes and then concentrated. The residue was diluted with 50 mL of methylene chloride and then concentrated via rotary evaporation. The residue was then diluted with 50 mL of methanol and re-concentrated via rotary evaporation. The residue was again re-diluted with 50 mL of methylene chloride and re-concentrated, first via rotary evaporation and then under full vacuum pump pressure (<0.5 mm Hg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07744853B2uspto-grants-2010_06