反应详情

温度

60 °C

Methyl 1-[methyl(N-{[(phenylmethyl)oxy]carbonyl}glycyl)amino]cyclopropanecarboxylate (3.66 g, 11.42 mmol) was dissolved in 50 mL of MeOH, degassed and placed under argon. 10% Pd/C (2.04 g) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon for 2 h. The contents were then degassed, and the Pd/C was removed by filtration through Celite, washing with MeOH. The filtrate was concentrated in vacuo. The residue was dissolved in MeOH (100 mL) and heated to 60° C. with stirring for 4 h. The solvent was removed in vacuo to provide pure 4-methyl-4,7-diazaspiro[2.5]octane-5,8-dione (1.76 g, 99%). LCMS: (M+H)+: 155.1.

1. customdegassed
2. addition10% Pd/C (2.04 g) was added
3. customthe contents were thoroughly degassed
4. customfor 2 h
5. customThe contents were then degassed
6. customthe Pd/C was removed by filtration through Celite
7. washwashing with MeOH
8. concentrationThe filtrate was concentrated in vacuo
9. dissolutionThe residue was dissolved in MeOH (100 mL)
10. customThe solvent was removed in vacuo