反应详情

660 mg (2 mmol) of 7-chloro-4,5-dihydro-3-(3-hydroxy-3-methyl-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepine-one was heated to boiling under reflux overnight with 80 mg of sodium hydroxide in 10 ml of toluene. After evaporation of the solvent the residue was dissolved in methylene chloride and the solution was washed twice with water, dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate there was obtained 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 200°-201°.

1. customAfter evaporation of the solvent the residue
2. dissolutionwas dissolved in methylene chloride
3. washthe solution was washed twice with water
4. dry with materialdried over magnesium sulphate
5. customevaporated
6. customAfter recrystallization of the residue from ethyl acetate