反应详情

Potassium hydroxide, 1.3 g (0.02 mole), was dissolved in 1 ml of water and added to a suspension of 4 g (0.0097 mole) of 8-chloro-6-(2-chlorophenyl)-1,2-dihydro-2-methyl-1-oxo-4H-imidazo [1,5-a] [1,4]benzodiazepin-3-carboxylic acid methyl ester ethanolate in 200 ml of methanol. The solution was refluxed under argon for 3 hrs, concentrated at reduced pressure, diluted with cold water and acidified with acetic acid to give an off-white solid. The solid was washed with water and air dried on the funnel overnight to give crude end product. Recrystallization from ethanol/methylene chloride gave white crystals with mp 265°-267° (dec).

1. temperatureThe solution was refluxed under argon for 3 hrs
2. concentrationconcentrated at reduced pressure
3. additiondiluted with cold water
4. customto give an off-white solid
5. washThe solid was washed with water and air
6. customdried on the funnel overnight
7. customto give crude end product
8. customRecrystallization from ethanol/methylene chloride
9. customgave white crystals with mp 265°-267° (dec)