Reaktion #706654

Reaktionsgleichung

3-methyl-2-[5-(amino)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene

triethylamine

pentafluoropropionic acid ethyl ester

→

desired compound

3-Methyl-2-[5-(pentafluoropropanoylamino)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONthe the solvent was distilled off
2. 2
   workup.ADDITIONTo the residue was added ethyl acetate
3. 3
   Waschenwashed with water
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent was distilled off
6. 6
   Sonstigethe residue was purified by column chromatography (eluent: ethyl acetate)
7. 7
   Sonstigeto afford 245 mg (58.1%

Vorschrift

To a solution of 275 mg (1.00 mmol) of 3-methyl-2-[5-(amino)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene in 30 ml of acetonitrile were added 0.19 ml (1.36 mmol) of triethylamine and 231 mg (1.20 mmol) of pentafluoropropionic acid ethyl ester. The mixture was stirred for 15 hours at room temperature, and the the solvent was distilled off. To the residue was added ethyl acetate, 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 245 mg (58.1%, a pale brown solid) of the desired compound.

Quelle