反应详情

4-(4-Hydroxy-7H-pyrrolo[2,3-d]pyrimidin-6-yl)-benzonitrile (2.36 g, 0.01 mol) are suspended in 40 ml acetonitril and 4.99 ml (0.02 mol) 4 N hydrochloric acid solution in dioxane. After addition of 3.66 ml (0.04 mol) phosphorus oxichloride the mixture is heated under reflux for 3 days. The solid is filtered off and the mother liquor evaporated. The residue and the solid are dissolved in 30 ml DMF at 60° C. and 25 ml of a conc. sodium bicarbonate solution and 25 ml water are added and the resulting suspension cooled, filtered and the solid washed with water. The title compound is dried at 100° C. for 6 h under reduced pressure; m.p. 296-297° C.; HPLC tR=11.59 min.

1. temperatureis heated
2. temperatureunder reflux for 3 days
3. filtrationThe solid is filtered off
4. customthe mother liquor evaporated
5. dissolutionThe residue and the solid are dissolved in 30 ml DMF at 60° C.
6. addition25 ml of a conc. sodium bicarbonate solution and 25 ml water are added
7. temperaturethe resulting suspension cooled
8. filtrationfiltered
9. washthe solid washed with water
10. dry with materialThe title compound is dried at 100° C. for 6 h under reduced pressure