反应详情

温度

80 °C

To a suspension of methyl N-{[3′-({[(4-oxo-3,4-dihydroquinazolin-2-yl)carbonyl]amino}methyl)biphenyl-4-yl]sulfonyl}valinate obtained in Reference Example 95 (0.250 g, 0.456 mmol) in THF (3 mL)-methanol (3 mL)-water (3 mL) was added 4N aqueous sodium hydroxide solution (0.399 mL, 1.60 mmol) at room temperature, and the mixture was stirred under heating at 80° C. for 15 hr. The reaction mixture was allowed to cool to room temperature, and concentrated under reduced pressure, and the residue was diluted with water. The mixture was acidified with 1N hydrochloric acid, and partitioned between ethyl acetate and water. The organic layer was washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from methanol to give the title compound as a white powder (0.202 g, 83%).

1. temperatureto cool to room temperature
2. concentrationconcentrated under reduced pressure
3. additionthe residue was diluted with water
4. custompartitioned between ethyl acetate and water
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customthe residue was crystallized from methanol