反应详情

温度

25 °C

42 ml of a 4% NaOH solution is added to a solution of 3.0 g of AgNO3 in water (50 ml). The solution of 3.0 g of 8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h-][2,3]-benzodiazepine in 120 ml of dioxane is slowly added to the heterogeneous mixture, and the reaction mixture is stirred for 30 minutes at 25° C. After activated carbon is added, it is filtered, the filtrate is concentrated by evaporation in a vacuum at 50-60° C., the suspension that is produced is diluted with 30 ml of water and cooled. After standing overnight, it is filtered off, the precipitate is washed with 2×10 ml of ice water, and 1.94 g of sodium salt, which is dissolved in 60 ml of hot water and, after cooling, acidified with 1 ml of acetic acid, is obtained. After filtration and washing with water, 1.66 g (53%) of product with a melting point of 196-198° C. (decomposition) is obtained.

1. additionAfter activated carbon is added
2. filtrationit is filtered
3. concentrationthe filtrate is concentrated by evaporation in a vacuum at 50-60° C.
4. customthe suspension that is produced
5. temperaturecooled
6. waitAfter standing overnight
7. filtrationit is filtered off
8. washthe precipitate is washed with 2×10 ml of ice water, and 1.94 g of sodium salt, which
9. dissolutionis dissolved in 60 ml of hot water
10. temperatureafter cooling
11. customis obtained
12. filtrationAfter filtration
13. washwashing with water, 1.66 g (53%) of product with a melting point of 196-198° C. (decomposition)
14. customis obtained