反应详情

温度

70 °C

A solution of 5-(8-chloro-2,6-dioxo-3-pentyl-2,3,6,7-tetrahydro-1H-purin-1-yl)pentanenitrile (3.0 g, 8.9 mmol) in EtOH (30 ml) was treated with water (15 ml), potassium carbonate (1.48 g, 10.7 mmol) and hydroxylamine hydrochloride (0.74 g, 10.7 mmol) and then heated at 70° C. overnight. A further potassium carbonate (1.5 g, 10.9 mmol) and hydroxylamine hydrochloride (1.0 g, 14.5 mmol) were cautiously added to the mixture which was then heated to 90° C. for 24 h. The mixture was cooled and concentrated in vacuo to remove most of the EtOH. The residual mixture was treated with water (30 ml) and acidified to pH 7 by the cautious addition of 2M aqueous hydrochloric acid. The precipitated solid was filtered off, washed with water, then with diethyl ether and thoroughly dried to yield the title compound as a white solid (2.80 g, 85%).

1. temperaturewas then heated to 90° C. for 24 h
2. temperatureThe mixture was cooled
3. concentrationconcentrated in vacuo
4. customto remove most of the EtOH
5. additionThe residual mixture was treated with water (30 ml)
6. additionacidified to pH 7 by the cautious addition of 2M aqueous hydrochloric acid
7. filtrationThe precipitated solid was filtered off
8. washwashed with water
9. dry with materialwith diethyl ether and thoroughly dried