反应详情

温度

20 °C

20 ml of 30% sodium hydroxide solution are added, at a temperature in the region of 20° C., to 1 g of 8-(3-ethoxycarbonylmethylureido)-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one in suspension in 40 ml of ethanol. The reaction is continued for 18 hours at 50° C. After cooling to a temperature in the region of 20° C., the precipitate formed is filtered, then taken up in 20 ml of distilled water and the mixture is acidified using concentrated hydrochloric acid. The suspension is stirred for 2 hours at a temperature in the region of 20° C. and then filtered, washed with water and dried under partial vacuum (1 mm Hg, 0.13 kPa) at 100° C. After recrystallization from dimethylformamide, there is obtained 0.22 g of 8-(3-carboxymethylureido)-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one dihydrate in the form of a beige solid, the melting point of which is greater than 260° C. (Analysis C16H12N5O4 2.0.H2O.0.1DMF, % calculated C: 56.64, H: 3.86, N: 20.64, % found C: 56.7, H: 3.8, N: 21.0).

1. customthe precipitate formed
2. filtrationis filtered
3. filtrationfiltered
4. washwashed with water
5. customdried under partial vacuum (1 mm Hg, 0.13 kPa) at 100° C
6. customAfter recrystallization from dimethylformamide