Reaktion #1155934

Reaktionsgleichung

3-methyl-1-[5-(amino)pentan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one

triethylamine

pentafluoropropionic acid ethyl ester

→

desired compound

Ausbeute 50.5%

3-Methyl-1-[5-(pentafluoropropanoylamino)pentan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one

Ausbeute 50.5%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture was stirred for 4 hours at the same temperature
2. 2
   workup.DISTILLATIONThe solvent was distilled off
3. 3
   workup.ADDITIONTo the residue was added methylene chloride
4. 4
   Waschenthe mixture was washed with water
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off
7. 7
   Sonstigethe residue was purified by column chromatography (eluent: ethyl acetate)

Vorschrift

To a solution of 2.58 g (10.0 mmol) of 3-methyl-1-[5-(amino)pentan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one and 1.81 ml (13.0 mmol) of triethylamine in 100 ml of acetonitrile was added, while stirring at room temperature, 2.31 g (12.0 mmol) of pentafluoropropionic acid ethyl ester. The mixture was stirred for 4 hours at the same temperature. The solvent was distilled off. To the residue was added methylene chloride, and the mixture was washed with water, and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: ethyl acetate) to afford 2.04 g of the desired compound (50.4%, a pale yellow solid).

Quelle