反应详情

Palladium (10% on carbon; 1.0 g) was added to a solution of benzyl 1-methyl-2,4-dioxo-1,3,8-triazaspiro[4.5]decane-8-carboxylate (7.82 g, 24.6 mmol) in ethanol (100 mL). The reaction vessel was evacuated and back-filled with nitrogen (3×), then back-filled with hydrogen (1 atm). After 2 h, methanol (50 mL) was added to the reaction mixture and the mixture was continued to be stirred under hydrogen (1 atm). After 4 days, the mixture was filtered through celite, washed with acetone and concentrated. The mixture was diluted in acetic acid (50 mL). The reaction vessel was evacuated and back-filled with nitrogen (3×), then back-filled with hydrogen (1 atm). After 2 h, the mixture was filtered through celite, and concentrated to give the acetate salt of the title compound (2.98 g). MS 184.1 (M+1).

1. customThe reaction vessel was evacuated
2. additionback-filled with nitrogen (3×)
3. additionback-filled with hydrogen (1 atm)
4. additionmethanol (50 mL) was added to the reaction mixture
5. waitAfter 4 days
6. filtrationthe mixture was filtered through celite
7. washwashed with acetone
8. concentrationconcentrated
9. additionThe mixture was diluted in acetic acid (50 mL)
10. customThe reaction vessel was evacuated
11. additionback-filled with nitrogen (3×)
12. additionback-filled with hydrogen (1 atm)
13. waitAfter 2 h
14. filtrationthe mixture was filtered through celite
15. concentrationconcentrated