반응 #1155934

반응 방정식

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

triethylamine

pentafluoropropionic acid ethyl ester

→

desired compound

수율 50.5%

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

수율 50.5%

용매

acetonitrile

반응 조건

후처리

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
   세척the mixture was washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off
7. 7
   기타the residue was purified by column chromatography (eluent: ethyl acetate)

실험 절차

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).

출처