反应详情

Sodium bicarbonate (0.058 g, 0.069 mmol) and 5% Pd/C (0.250 g, Johnson Matthey Type 440 paste) were added to a solution of [2-(7-benzyl-9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl)ethyl]carbamic acid tert-butyl ester (see Example I (Alternative I) above; 1 g, 2.77 mmol) in ethanol (10 mL). The mixture was then hydrogenated at 500 kPa (5 bar) for 18 hours. The reaction mixture was filtered through Celite® and then washed with ethanol (20 mL). The solution was concentrated under reduced pressure to give an oil. This was dissolved in dichloromethane (20 mL) and washed with sodium hydroxide (1 M, 10 mL). The organic phase was separated, dried over magnesium sulfate and then filtered. The filtrate was concentrated under reduced pressure to give the title compound as a yellow solid (0.67 g, 87%).

1. filtrationThe reaction mixture was filtered through Celite®
2. washwashed with ethanol (20 mL)
3. concentrationThe solution was concentrated under reduced pressure
4. customto give an oil
5. washwashed with sodium hydroxide (1 M, 10 mL)
6. customThe organic phase was separated
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. concentrationThe filtrate was concentrated under reduced pressure