反应详情

A sample of benzyl (S)-1-((1S,2R,4R)-2-acetamido-4-((4-methoxybenzyl)(methyl)amino)cyclohexyl)-2-oxopyrrolidin-3-ylcarbamate (25.0 g, 47.8 mmol) was dissolved in MeOH. The flask was charged with dihydroxypalladium (6 g, 8.54 mmol), evacuated, and back filled with hydrogen from a hydrogen balloon. The mixture was stirred at RT overnight and then filtered (3×80 mL isopropanol washes). The residue was concentrated under high vacuum to dryness. The residue was dried azeotropically with iso-propanol (4×150 mL) under reduced pressure to afford N-((1R,2S,5R)-2-((S)-3-amino-2-oxopyrrolidin-1-yl)-5-(methylamino)cyclohexyl)acetamide (12.5 g, 46.6 mmol, 97% yield). LC/MS found [M+H]+=269.

1. customevacuated
2. additionback filled with hydrogen from a hydrogen balloon
3. filtrationfiltered (3×80 mL isopropanol washes)
4. concentrationThe residue was concentrated under high vacuum to dryness
5. dry with materialThe residue was dried azeotropically with iso-propanol (4×150 mL) under reduced pressure