反应详情

3,4-di(prop-1-en-2-yl)dibenzo[b,d]furan-1-amine (4.8 g, 18.2 mmol), and 5% Pt/C (0.48 g) and 10% Pd/C (0.48 g) were added to a mixture of ethanol (90 mL) and acetic acid (10 mL). Reaction mixture was hydrogenated overnight at 50 psi. Reaction mixture was filtered through a Celite pad and most of the organic solvent was evaporated under vacuum. Crude product was dissolved in ethylacetate and partitioned between 1N NaOH and ethylacetate to get rid of any acetic acid. Organic layer was dried over anhydrous Na2SO4, evaporated under vacuum and purified by flash chromatography over silica gel with 40% DCM/hexanes. Target compound (3.3 g, 68%) was isolated as white crystals.

1. customReaction mixture
2. customReaction mixture
3. filtrationwas filtered through a Celite pad and most of the organic solvent
4. customwas evaporated under vacuum
5. dissolutionCrude product was dissolved in ethylacetate
6. custompartitioned between 1N NaOH and ethylacetate
7. customto get rid of any acetic acid
8. dry with materialOrganic layer was dried over anhydrous Na2SO4
9. customevaporated under vacuum
10. custompurified by flash chromatography over silica gel with 40% DCM/hexanes