反应详情

Compound 37e (450 mg, 1.02 mmol) was added to a 500 mL-Parr hydrogenation bottle and dissolved in absolute EtOH (6 mL). A 12N conc. HCl solution (95 μL, 1.14 mmol) was added and the bottle was purged with N2. 10% Pd/C (264 mg) was added and the mixture was shaken under 60 psi of H2 for 14 h. An additional amount of 10% Pd/C (430 mg) was added and the mixture was returned to 60 psi of H2 and shaken 5 h more. The mixture was filtered through a pad of diatomaceous earth, and the solids were rinsed thoroughly with MeOH. The fitrate was concentrated to dryness under reduced pressure to afford crude compound 37f as a sticky oil (428 mg) which was used in the following step without further purification. LC/MS m/z (M+H+) 276.3.

1. customthe bottle was purged with N2
2. addition10% Pd/C (264 mg) was added
3. additionAn additional amount of 10% Pd/C (430 mg) was added
4. stirringshaken 5 h more
5. filtrationThe mixture was filtered through a pad of diatomaceous earth
6. washthe solids were rinsed thoroughly with MeOH
7. concentrationThe fitrate was concentrated to dryness under reduced pressure