反应详情

To the product from Method B (0.7 grams, 2.19 mmol) dissolved in 15 mL of ethanol was added 1.5 mL of 2 N hydrochloric acid and the reaction mixture degassed by nitrogen purge. To the reaction mixture was then added 0.5 grams of 20% palladium hydroxide on carbon (50% water) (Aldrich) and the resulting mixture shaken (Parr-Shaker) under a 50 psi atmosphere of hydrogen at room temperature for 2 days. The Celite filtered reaction mixture was concentrated to dryness in vacuo and the residue purified by flash chromatography (silica; 5% methanol in dichloromethane) affording 0.48 grams (90%) of the title compound. LRMS: 246.1 (M+1).

1. customthe reaction mixture degassed by nitrogen
2. custompurge
3. additionTo the reaction mixture was then added 0.5 grams of 20% palladium hydroxide on carbon (50% water) (Aldrich)
4. filtrationThe Celite filtered
5. customreaction mixture
6. concentrationwas concentrated to dryness in vacuo
7. customthe residue purified by flash chromatography (silica; 5% methanol in dichloromethane)