反应详情

Trans-4-chloro-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidine (0.89 g, 1.9 nmol) in concentrated ammonium hydroxide (40 mL) and dioxane (40 mL) was heated at 120° C. in a pressure vessel for 18 hours. The mixture was allowed to cool to ambient temperature and the solvent was removed under reduced pressure. The residue was partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate. The water phase was further extracted with ethyl acetate and the combined organic extracts were washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to yield trans-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.35 g, 0.8 mmol). RP-HPLC (Hypersil C18, 5 μm, 250×4.6 mm; 25%-100% over 15 min with 0.1 M ammnonium acetate, 1 mL/min) Rt 4.01 min. MS: MH+441.

1. customthe solvent was removed under reduced pressure
2. customThe residue was partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate
3. extractionThe water phase was further extracted with ethyl acetate
4. washthe combined organic extracts were washed with brine
5. dry with materialdried over sodium sulfate
6. customThe solvent was removed under reduced pressure