反应详情

Add 45 g of iron powder to a solution of 15 g (62.7 mmol) of the product from Example 19 in 400 ml of 75% acetic acid. Heat to 60°-70° C. for 2 hr. Filter the reaction mixture over celite and concentrate the filtrate to approximately 50 ml under vacuum. Neutralize the residue with saturated sodium carbonate solution and extract with three 200 ml portions of methylene chloride. Dry the combined extracts over sodium sulfate, treat with charcoal and remove the solvent in vacuo. Crystallize the residue from ether to provide the title compound.

1. temperatureHeat to 60°-70° C. for 2 hr
2. filtrationFilter the reaction mixture over celite and
3. concentrationconcentrate the filtrate to approximately 50 ml under vacuum
4. extractionNeutralize the residue with saturated sodium carbonate solution and extract with three 200 ml portions of methylene chloride
5. dry with materialDry the combined extracts over sodium sulfate
6. additiontreat with charcoal
7. customremove the solvent in vacuo
8. customCrystallize the residue from ether