反应详情

A solution of 2 g (0.005 mole) of 6-(2-chlorophenyl)-1,8-dichloro-4H-imidazo[1,5-a] [1,4]benzodiazepine-3-carboxylic acid, methyl ester 0.7 g (0.012 mole) of potassium hydroxide, 60 ml of methanol and 2 ml of water was refluxed under argon for 2.5 hrs. The solution was evaporated in vacuo at 50°-60°. An aqueous solution of the residue was acidified with acetic acid to give a gelatinous, white precipitate. The precipitate was collected by filtration, washed with water and air dried on the funnel overnight to give off-white solid. Recrystallization from a solution of ethanol and methylene chloride gave white plates with mp 250°-253° (dec).

1. customThe solution was evaporated in vacuo at 50°-60°
2. customto give a gelatinous, white precipitate
3. filtrationThe precipitate was collected by filtration
4. washwashed with water and air
5. customdried on the funnel overnight
6. customto give off-white solid
7. customRecrystallization from a solution of ethanol and methylene chloride
8. customgave white plates with mp 250°-253° (dec)