反应详情

温度

5 °C

4.1. 77 g of 5-(chloromethyl)-1,2,4-triazolo[4,3-c]quinazoline are suspended in 2.0 l of acetone (or dioxan) and cooled to 5° C. 410 ml of 1N sodium hydroxide solution are added in such a manner that the temperature rises to about 13° C. The mixture is stirred at room temperature for 17 h. The reaction mixture is then made slightly acidic (pH 6) with 3N hydrochloric acid and concentrated in a vacuum. The crystalline precipitate is filtered off, washed and dried. There are obtained 65 g of crude 5H-[1,2,4]triazolo[1,5-d][1,4]benzodiazepin-6(7H)-one. The filtrate is saturated with sodium chloride and extracted 3 times with 0.51 of dichloromethane each time. The organic phases are evaporated in a vacuum. 12 g of crude 5H-[1,2,4]triazolo[1,5-d][1,4]benzodiazepin-6(7H)-one are obtained. Both crude crystallizates (77 g) are dissolved together in 5 l of dichloromethane and 250 ml of ethanol at reflux temperature. A small insoluble constituent is separated by filtration, the filtrate is cooled to room temperature and filtered through a column of 1500 g of silica gel. The column is rinsed with a mixture of 5.7 l of dichloromethane and 0.3 l of ethanol. After concentrating all eluates, there are obtained 62 g of yellow crystals. These are stirred at reflux temperature as a suspension in 600 ml of ethyl acetate and then cooled to 0° C. The crystals are filtered off, washed with diethyl ether and dried. There are obtained 51 g of 5H-[1,2,4]triazolo[1,5-d][1,4]benzodiazepin-6(7H)-one of m.p. 223°-223° C.

1. customrises to about 13° C
2. concentrationconcentrated in a vacuum
3. filtrationThe crystalline precipitate is filtered off
4. washwashed
5. customdried