反应 #1328400

ord-2f811d3503804301b689162b61a2ec69

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07115248B2uspto-grants-2006_10