反应详情

A mixture of 2-butyl-5-cyano-4-(1H-pyrrol-1-yl)-1-[(2'-(1H-tetrazol-5-yl)biphen-4-yl)methyl]-1H-imidazole (Example 15, 1.4 g) and 2 N NaOH (75 mL) was heated at reflux for 24 hours. The cooled solution was acidified to pH 3.5 by portionwise addition of citric acid. The resulting precipitate was collected by filtration and rinsed well with water. The solid was then purified by C18 -reversed phase chromatography eluting with acetonitrile-water (40:60). The majority of the acetonitrile was evaporated from the pure fractions at reduced pressure, keeping the temperature below 30° C. The remaining aqueous portion was washed with ethyl acetate and the organic layer was dried over anhydrous magnesium sulfate and evaporated. The residue was dissolved in ether and evaporated once again to give the title compound as a colorless powder. MS (FAB, thioglycerol) 468 (m+1), 424 (m-CO2 +1).

1. temperaturewas heated
2. temperatureat reflux for 24 hours
3. filtrationThe resulting precipitate was collected by filtration
4. washrinsed well with water
5. customThe solid was then purified by C18 -reversed phase chromatography
6. washeluting with acetonitrile-water (40:60)
7. customThe majority of the acetonitrile was evaporated from the pure fractions at reduced pressure
8. customthe temperature below 30° C
9. washThe remaining aqueous portion was washed with ethyl acetate
10. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
11. customevaporated
12. dissolutionThe residue was dissolved in ether
13. customevaporated once again