反应详情

500 mg of ethyl 4-(1-hydroxy-1-methylethyl)-2-methylthio-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in Example 105(b)] and 131 mg of lithium hydroxide monohydrate were added to a mixture of 5 ml of water and 5 ml of dioxane, and the resulting mixture was stirred at room temperature for 24 hours. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure, and the resulting residue was dissolved in water. 3.1 ml of 1N aqueous hydrochloric acid were then added, and the crystals which appeared were collected by filtration. These crystals were dissolved in ethyl acetate, and water was added to induce crystallization. The crystals which appeared were collected by filtration and washed with ethyl acetate and water, to give 290 mg of the title compound as crystals, melting at 169°-171° C. (with decomposition).

1. concentrationAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
2. dissolutionthe resulting residue was dissolved in water
3. addition3.1 ml of 1N aqueous hydrochloric acid were then added
4. filtrationthe crystals which appeared were collected by filtration
5. dissolutionThese crystals were dissolved in ethyl acetate
6. additionwater was added
7. customcrystallization
8. filtrationThe crystals which appeared were collected by filtration
9. washwashed with ethyl acetate and water