反应详情

温度

120 °C

A mixture of N-[4-(4-chloro-7-isopropylpyrrolo[2,3-d]pyrimidin-5-yl)phenyl]-benzenesulphonamide (0.34 g), concentrated ammonia (30 ml, SG 0.880) and 1,4-dioxane (30 ml) was heated with stirring at 120° C. in a pressure vessel for 16 hours. The mixture was allowed to cool to ambient temperature and the solvent was removed under reduced pressure to give a residue which was partitioned between water (40 ml) and ethyl acetate (40 ml). The organic layer was separated and the aqueous layer was further extracted with ethyl acetate (2×40 ml). The combined ethyl acetate extracts were washed, dried, filtered and evaporated to give a solid which was purified by flash column chromatography on silica using ethyl acetate/cyclohexane (8:2) as the mobile phase. Appropriate fractions were collected, combined and concentrated to give N-[4-(4-amino-7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)phenyl]benzenesulphonamide, m.p. 238-240° C.

1. temperaturewas heated
2. temperatureto cool to ambient temperature
3. customthe solvent was removed under reduced pressure
4. customto give a residue which
5. customwas partitioned between water (40 ml) and ethyl acetate (40 ml)
6. customThe organic layer was separated
7. extractionthe aqueous layer was further extracted with ethyl acetate (2×40 ml)
8. washThe combined ethyl acetate extracts were washed
9. customdried
10. filtrationfiltered
11. customevaporated
12. customto give a solid which
13. customwas purified by flash column chromatography on silica
14. customAppropriate fractions were collected
15. concentrationconcentrated