反应详情

A mixture of 6-(2-dimethylamino-ethoxy)-3,4-dihydro-2H-naphthalen-1-one oxime (0.3 g, 1.2 mmol), EtOH (12 mL), Pd/C (Aldrich, 0.13g, 0.12 mmol), and concentrated HCl (0.24 mL) was purged with H2 and connected to a H2 balloon overnight at RT. The catalyst was filtered through Celite® and washed with MeOH. The filtrate was concentrated in vacuo. The residue was added saturated NaHCO3 and extracted with CH2Cl2. The organic solution was dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by silica gel chromatography (5%-10% MeOH—CH2Cl2) to afford the compound as a colorless oil. MS (ESI): 235 (M+H)+.

1. customwas purged with H2
2. customconnected to a H2 balloon overnight at RT
3. filtrationThe catalyst was filtered through Celite®
4. washwashed with MeOH
5. concentrationThe filtrate was concentrated in vacuo
6. additionThe residue was added saturated NaHCO3
7. extractionextracted with CH2Cl2
8. dry with materialThe organic solution was dried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customThe crude product was purified by silica gel chromatography (5%-10% MeOH—CH2Cl2)