反应详情

A solution containing ethyl 4-[3-(1H-imidazol-1-yl)-2-[[(4-methoxyphenyl)methoxy]methyl]-1E-propenyl]benzoate (prepared as in Example 1; 0.7 g, 0.0017 mol) in ethanol (10 ml) was treated with aqueous sodium hydroxide (3.5 ml of 1M). The resulting mixture was stirred at room temperature for 5 hours after which time the solvent was evaporated off under reduced pressure and the resulting residue was dissolved in water (100 ml) and washed with ethyl acetate. The aqueous solution was acidified to pH 6.5 with hydrochloric acid and extracted with ethyl acetate (3×150 ml). The extracts were combined, dried over sodium sulfate, and the solvent was evaporated off under reduced pressure to yield a crude product. The crude product was recrystallised from dichloromethane-pentane to yield 4-[3-(1H-imidazol-1-yl)-2-[[(4-methoxyphenyl)methoxy]methyl]-1E-propenyl]benzoic acid as a colourless, crystalline solid, having a melting point of 120°-122° C. and the following structural characteristics:

1. customwas evaporated off under reduced pressure
2. dissolutionthe resulting residue was dissolved in water (100 ml)
3. washwashed with ethyl acetate
4. extractionextracted with ethyl acetate (3×150 ml)
5. dry with materialdried over sodium sulfate
6. customthe solvent was evaporated off under reduced pressure
7. customto yield a crude product
8. customThe crude product was recrystallised from dichloromethane-pentane