Reaktion #1854216

Reaktionsgleichung

Fmoc-Lys(MMT)

methylene chloride

diethylamine

Lys

Fmoc-Lys(MMT)

→

Lys(MMT)

Lösungsmittel

acetonitrile

—

mixture

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter removal of solvent
2. 2
   Sonstigethe residue was flushed with acetonitrile at 60° C. (90 ml×2)
3. 3
   Waschenwashed with acetonitrile (20 ml×3) and ether (20 ml×3)
4. 4
   workup.DISSOLUTIONThe solid was then dissolved as far as possible in 1:1 CH2Cl2/CH3OH (200 ml)
5. 5
   Sonstigesome solid byproduct was removed
6. 6
   Filtrationby filtering
7. 7
   Filtrationthrough filter paper
8. 8
   SonstigeAfter removal of solvent
9. 9
   Sonstigebeing dried in vacuo, 4.7707 g (82.2%, based on Fmoc-Lys) of pale yellow foam
10. 10
    Sonstigewas obtained

Vorschrift

To a stirred solution of Fmoc-Lys(MMT) (9.7336 g) in 100 ml of mixture of methylene chloride and acetonitrile (1:1) at room temperature was added diethylamine (100 ml). The mixture was stirred at room temperature for 1.5 hrs. After removal of solvent, the residue was flushed with acetonitrile at 60° C. (90 ml×2), washed with acetonitrile (20 ml×3) and ether (20 ml×3). The solid was then dissolved as far as possible in 1:1 CH2Cl2/CH3OH (200 ml) and some solid byproduct was removed by filtering through filter paper. After removal of solvent and being dried in vacuo, 4.7707 g (82.2%, based on Fmoc-Lys) of pale yellow foam was obtained. ES(+)-MS: 147(Lys+1), 273(MMT).

Quelle