(8aR)-2-benzyl-1,3,4,7,8,8a-hexahydropyrrolo[1,2-a]pyrazin-6-one

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of (R)-(+)-2-benzylhexahydropyrrolo[1,2-a]pyrazin-6(7H)-one (2 g, 8.69 mmol), ammonium formate (3.83 g, 60.8 mmol) and 10% Pd/C (550 mg) in MeOH (90 ml) was refluxed for 3 hours. After cooling to room temperature, the catalyst was filtered off and the solvent evaporated under vacuum. The residue was purified by flash chromatography (DCM/MeOH/32% NH4OH, 70/30/3 respectively) to afford the title compound as a colourless oil (1.1 g, 90% yield). was refluxed for 3 hours the catalyst was filtered off the solvent evaporated under vacuum The residue was purified by flash chromatography (DCM/MeOH/32% NH4OH, 70/30/3 respectively)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methanesulfonic acid 2-[benzyl-((R)-5-oxo-pyrrolidin-2-ylmethyl)-amino]-ethyl ester (3.5 g, 10.74 mmol) was dissolved in CH3CN (20 ml) and then 60% NaH (558 mg, 13.96 mmol) was added portionwise at room temperature. After stirring for 4 hours, the solvent was removed under vacuum and the residue was treated with water and extracted with ethyl acetate. The organic phase was washed with brine, dried (Na2SO4) and evaporated under vacuum. The residue was purified by flash chromatography (DCM/abs EtOH/Petroleum Ether/33% NH4OH/Et2O 300/180/900/9.9/360 respectively) to afford the title compound as yellow oil (2.1 g, 85% yield). the solvent was removed under vacuum the residue was treated with water extracted with ethyl acetate The organic phase was washed with brine dried (Na2SO4) evaporated under vacuum The residue was purified by flash chromatography (DCM/abs EtOH/Petroleum Ether/33% NH4OH/Et2O 300/180/900/9.9/360 respectively)