反应详情

温度

0 °C

To a suspension of sodium hydride (60% oil suspension, 154 mg) in tetrahydrofuran (4 ml) was added a solution of 5-(4-nitrobenzoyl)-1,3,4,5-tetrahydro-1,5-benzodiazepin-2(2H)-one (800 mg) in tetrahydrofuran (6 ml) at 0° C. and the mixture was stirred at 0° C. for 5 minutes. To the mixture was added ethyl bromoacetate (472 mg) and then the mixture was stirred at ambient temperature overnight. The reaction was quenched with saturated ammonium chloride aqueous solution and the resultant mixture was diluted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate aqueous solution and brine, and then it was dried over magnesium sulfate. Filtration and evaporation afforded 1-ethoxycarbonylmethyl-5-(4-nitrobenzoyl)-1,3,4,5-tetrahydro-1,5-benzodiazepin-2(2H)-one (691 mg) as a slightly yellow amorphous.

1. stirringthe mixture was stirred at ambient temperature overnight
2. customThe reaction was quenched with saturated ammonium chloride aqueous solution
3. additionthe resultant mixture was diluted with ethyl acetate
4. washThe organic layer was washed with saturated sodium bicarbonate aqueous solution and brine
5. dry with materialit was dried over magnesium sulfate
6. filtrationFiltration and evaporation