反应详情

1-[1-(2-Thenoylmethyl)-2-oxo-5-pivaloyl-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(3-ethoxycarbonylphenyl)urea (0.67 g) was suspended in a mixed solvent of ethanol (10 ml) and tetrahydrofuran (10 ml), aqueous lithiumhydroxide monohydrate (0.24 g) solution (10 ml) was added, and the mixture was stirred for 3 hours at room temperature. The reaction mixture was concentrated under reduced pressure, weakly acidified with 1N hydrochloric acid, extracted with methylene chloride. The organic layer was successively washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, the residue was suspended in a mixed solvent of methanol and ethyl acetate, crystals so precipitated were collected by filtration, to thereby obtain 0.48 g of the titled compound as white crystals (Yield: 78%).

1. additionwas added
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. extractionextracted with methylene chloride
4. washThe organic layer was successively washed with water and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customso precipitated
8. filtrationwere collected by filtration