反应详情

A mixture of 7-isopropyl-5-[4-(2-nitrophenoxy)phenyl]-7H-pyrrolo[2,3-d]-pyrimidin-4-ylamine (0.15 g), ammonium formate (3 equivalents), 10% palladium on charcoal (15 mg) and ethanol (5 ml) was boiled under reflux under nitrogen for 2 hours. Further ammonium formate (100 mg) was added after one hour. The mixture was cooled and filtered through silica. The filter bed was washed with industrial methylated spirit (2×10 ml). The filtrate was evaporated and the residue was extracted with ethyl acetate. The ethyl acetate was removed under reduced pressure to give a residue which was purified by flash column chromatography on silica using ethyl acetate as the mobile phase to give 5-[4-(2-aminophenoxy)phenyl]-7-isopropyl-7H-pyrrolo[2,3-d]-pyrimidin-4-ylamine. The structure was confirmed by 1H nmr.

1. temperatureunder reflux under nitrogen for 2 hours
2. temperatureThe mixture was cooled
3. filtrationfiltered through silica
4. washThe filter bed was washed with industrial methylated spirit (2×10 ml)
5. customThe filtrate was evaporated
6. extractionthe residue was extracted with ethyl acetate
7. customThe ethyl acetate was removed under reduced pressure
8. customto give a residue which
9. customwas purified by flash column chromatography on silica