反应详情

Compound 47 (0.060 g, 0.266 mmol) was diluted in absolute EtOH (7 mL) and methanolic ammonia (7 N, 7 mL) was added. Raney nickel (˜1.5 g, washed with H2O and MeOH) was added, and the mixture was degassed and hydrogenated with a balloon at room temperature for 30 min while stirring rapidly. The clear solution was decanted away from the nickel and was filtered through a Pall 0.2 μm syringe filter to remove fine particulate matter. The solution was concentrated and dried in vacuo to yield a colorless gum that became a white semisolid upon standing (0.050 g, 82%). Conversion to this amine was confirmed by 1H NMR spectrometry, TLC, MS, and ninhydrin staining, and it was used crude without any further characterization or purification.

1. customthe mixture was degassed
2. customThe clear solution was decanted away from the nickel
3. filtrationwas filtered through a Pall 0.2 μm syringe
4. filtrationfilter
5. customto remove fine particulate matter
6. concentrationThe solution was concentrated
7. customdried in vacuo
8. customto yield a colorless gum that
9. customwithout any further characterization or purification