反应详情

To a suspension of sodium hydride (0.185 g of a 60% dispersion in mineral oil) in dry N,N-dimethylformamide (5 ml) was added (3RS)-2,3-dihydro-5-(2-fluorophenyl)-3-phtalimido-1H-1,4-benzodiazepin-2-one (1.700 g) under stirring at cooling in an ice-bath. The mixture was stirred under the same condition for 1 hour and then at room temperature for 1.5 hours. To the mixture was added dropwise a solution of 2-bromomethylbenzofuran (1.076 g) in N,N-dimethylformamide (5 ml) under cooling in an ice-bath. After completion of the addition, the mixture was allowed to stand to room temperature overnight. The reaction mixture was concentrated in vacuo. The residue was treated with ethyl acetate and water. The organic layer was washed with water and a brine, and dried over magnesium sulfate. Removal of the solvent gave (3RS)-1-(benzofuran-2-yl)methyl-2,3-dihydro-5-(2-fluorophenyl)-3-phthalimido-1H-1,4-benzodiazepin-2-one (1.018 g) which was used in a following reaction step without further purification.

1. temperatureat cooling in an ice-bath
2. stirringThe mixture was stirred under the same condition for 1 hour
3. temperatureunder cooling in an ice-bath
4. additionAfter completion of the addition
5. waitto stand to room temperature overnight
6. concentrationThe reaction mixture was concentrated in vacuo
7. additionThe residue was treated with ethyl acetate and water
8. washThe organic layer was washed with water
9. dry with materiala brine, and dried over magnesium sulfate
10. customRemoval of the solvent