反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
On the other hand, to a suspension of (3S)-3-amino-1,3-dihydro-5-phenyl-1-[(1H-tetrazol-5-yl) methyl]-2H-1,4-benzodiazepin-2-one hydrochloride in dry dichloromethane (50 ml) was added dropwise triethylamine (7.45 ml). To the mixture was added dropwise a solution of 2-indolylcarbonyl chloride obtained above under stirring and cooling below 10° C. After stirring under the same conditions for 2 hours, the mixture was washed with hydrochloric acid, water and brine. The organic layer was dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethanol to give (3S)-1,3-dihydro-3-(2-indolylcarbonylamino)-5-phenyl-1-[(1 H-tetrazol-5-yl)-methyl]-2H-1,4-benzodiazepin-2-one (5.3 g).
WORKUP
后处理
- customobtained above
- temperaturecooling below 10° C
- stirringAfter stirring under the same conditions for 2 hours
- washthe mixture was washed with hydrochloric acid, water and brine
- dry with materialThe organic layer was dried over magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was recrystallized from ethanol