反应详情

温度

120 °C

A mixture of 4-(4-chloro-7-cyclopentyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-2-methoxyaniline (0.45 g, 1.31 mmol), ammonia (115 ml, SG 0.88) and 1,4-dioxane (115 ml) was heated and stirred at 120° C. in a pressure vessel overnight. 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 and ethyl acetate. The organic layer was separated and the aqueous layer was further extracted with ethyl acetate twice. The combined ethyl acetate extracts were washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered and evaporated to give 5-(4-amino-3-methoxyphenyl)-7-cyclopentyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine as brown solids (0.32 g, 0.99 mmol): 1H NMR (DMSO-d6, 400 MHz) δ 8.09 (s, 1H), 7.24 (s, 1H), 6.88 (d, 1H), 6.79 (dd, 1H), 6.71 (d, 1H), 6.01 (broad, 2H), 5.06 (m, 1H), 4.79 (broad, 2H), 3.81 (s, 3H), 2.10 (m, 2H), 1.87-1.92 (m, 4H), 1.68 (m, 2H); MH+324.

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 and ethyl acetate
6. customThe organic layer was separated
7. extractionthe aqueous layer was further extracted with ethyl acetate twice
8. washThe combined ethyl acetate extracts were washed with saturated aqueous sodium chloride solution
9. dry with materialdried over magnesium sulfate
10. filtrationfiltered
11. customevaporated