反应详情

4-Pentynoic acid (1.03 g) and N-methylpiperazine (1.0 g) was dissolved in 30 mL of DMF, 1.6 g of HOBt was added to the solution at ice temperature under stirring. After the mixture was stirred at same temperature for 15 minutes, additionally 2.3 g of WSC was added, and the solution was stirred at room temperature overnight. The DMF was removed under reduced pressure from the reaction mixture, then water was added to the residue and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and then the solvent was removed. The residue was purified by chromatography on silica gel (methylene chloride-methanol-triethylamine 600:20:1) to give 510 mg of 1-(4-methylpiperazin-1-yl)pent-4-yn-1-one as a colorless oil.

1. stirringAfter the mixture was stirred at same temperature for 15 minutes
2. stirringthe solution was stirred at room temperature overnight
3. customThe DMF was removed under reduced pressure from the reaction mixture
4. additionwater was added to the residue
5. extractionthe mixture was extracted with ethyl acetate
6. washThe organic layer was washed with brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was removed
9. customThe residue was purified by chromatography on silica gel (methylene chloride-methanol-triethylamine 600:20:1)