反应详情

A suspension of 40.0 g (83.9 mmol) of methyl-4-[(2-Butyl-5-formyl-4-iodo-1H-imidazol-1-yl)methyl]naphthalene-1-carboxylate, 9.07 g (92.4 mmol) of potassium acetate, and 6.0 g of 10% palladium on carbon in 1.2 liters of ethyl acetate was hydrogenated for 2 hours. The solids were removed by filtration and an additional 8.0 g of 10% palladium on carbon and 9.01 g (92.4 mmol) of potassium acetate was added. After hydrogenating the reation mixture an additional 2 hours, the solids were removed by filtration and the solution was concentrated to about 1/3 volume. The ethyl acetate solution was washed with aqueous sodium carbonate solution, dried over magnesium sulfate, and concentrated under vacuum to give an oil which crystallized. Recrystallization from methylene chloride-hexane gave 25.77 g (87.6%) of colorless crystals; mp 95.5°-97° C.

1. customThe solids were removed by filtration
2. customan additional 2 hours
3. customthe solids were removed by filtration
4. concentrationthe solution was concentrated to about 1/3 volume
5. washThe ethyl acetate solution was washed with aqueous sodium carbonate solution
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under vacuum
8. customto give an oil which
9. customcrystallized
10. customRecrystallization from methylene chloride-hexane