反应详情

In THF (4.5 ml)/ethanol (4.5 ml) was dissolved methyl 1-(allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate (0.30 g). To the solution was added 1N sodium hydroxide (3.0 ml), and the mixture was stirred at room temperature for 4 hours. pH was adjusted to approximate 4 with 1N hydrochloric acid, and the solvent was concentrated to half under reduced pressure. The concentrated material was extracted with ethyl acetate, the extract was washed with saturated brine and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was washed with hexane/ethyl acetate (=8/1) to give 1-(allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylic acid (0.25 g).

1. concentrationthe solvent was concentrated to half under reduced pressure
2. extractionThe concentrated material was extracted with ethyl acetate
3. washthe extract was washed with saturated brine
4. dry with materialdried with magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. washthe resulting residue was washed with hexane/ethyl acetate (=8/1)