反应详情

To a solution of diethyl 2,5-dioxo-4-imidazolylphosphonate (1.5 g, 0.33 mmol) in DMF (4 mL) is added K2CO3 and then 1-iodobutane (0.79 mL, 6.96 mmol). This mixture is stirred for 16 hours at room temperature. To this yellow mixture is added methyl 4-[(2-butyl-5-formyl-1H-imidazol-1-yl)methyl]benzoate (1.05 g, 3.5 mmol). After 2 hours methylene chloride (10 mL) was added to aid stirring. The mixture was stirred for 16 hours. After diluting the reaction mixture with water it was extracted with ethyl acetate. This extract was washed with water and brine. The extract was dried over MgSO4, filtered and then concentrated until crystallization was apparent. The solid was collected and dried.

1. stirringstirring
2. stirringThe mixture was stirred for 16 hours
3. extractionwas extracted with ethyl acetate
4. washThis extract was washed with water and brine
5. dry with materialThe extract was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated until crystallization
8. customThe solid was collected
9. customdried