Reaktion #47714

Reaktionsgleichung

N—BOC—N,N-bis-(N′,N′-bis(5-methoxycarbonylpentyl)-5-carbamyl pentyl)-amine

N—BOC—N,N-Bis-(N′,N′-Bis(5-Methoxycarbonylpentyl)-5-Carbamyl pentyl)Amine

trifluoroacetic acid

→

N,N-Bis-(N′,N′-Bis(5-Methoxycarbonylpentyl)-5-carbamyl pentyl)-Amine TFA

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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).

Quelle