Реакция #1328400

ord-2f811d3503804301b689162b61a2ec69

Уравнение реакции

COC(=O)CCCCCN(CCCCCC(=O)OC)C(=O)CCCCCN(CCCCCC(=O)N(CCCCCC(=O)OC)CCCCCC(=O)OC)C(=O)OC(C)(C)C
N-BOC-N,N-bis-(N′,N′-bis(5-methoxycarbonylpentyl)-5-carbamyl pentyl)-amine
COC(=O)CCCCCN(CCCCCC(=O)OC)C(=O)CCCCCN(CCCCCC(=O)N(CCCCCC(=O)OC)CCCCCC(=O)OC)C(=O)OC(C)(C)C
N-BOC-N,N-Bis-(N′,N′-Bis(5-Methoxycarbonylpentyl)-5-Carbamyl pentyl)Amine
O=C(O)C(F)(F)F
trifluoroacetic acid
COC(=O)CCCCCN(CCCCCC(=O)OC)C(=O)CCCCCNCCCCCC(=O)N(CCCCCC(=O)OC)CCCCCC(=O)OC.O=C(O)C(F)(F)F
N,N-Bis-(N′,N′-Bis(5-Methoxycarbonylpentyl)-5-carbamyl pentyl)-Amine TFA

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07115248B2uspto-grants-2006_10