반응 #706654

반응 방정식

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

용매

acetonitrile

반응 조건

후처리

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

실험 절차

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.

출처