反应详情

温度

120 °C

To a solution of 1-(phenylsulfonyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-amine in anhydrous dimethylacetamide (1 mL) was added 4-chloro-1H-pyrazolo[3,4-d]pyrimidin-6-amine (135 mg, 1.0 mmol) and diisopropylethylamine (0.4 mL, 2.30 mmol). The mixture was stirred at 120° C. for 20 hours. After cooling to room temperature the mixture was poured into water (10 ml) and extracted with ethyl acetate (3×10 ml). The combined organics were dried over sodium sulfate and concentrated to a residue which was purified by reverse phase chromatography on a preparative LC/UV/MS system using a mass triggered fractionation. Compounds were eluted from the HPLC column (Maccel 120-10-C18 SH 10 μm 20 mmID×50 mm) at 88 ml/min with 5-95 acetonitrile/water gradient using 0.1% TFA as modifier to yield N4-(1-(phenylsulfonyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-yl)-1H-pyrazolo[3,4-d]pyrimidine-4,6-diamine (13.4 mg).

1. temperatureAfter cooling to room temperature the mixture
2. extractionextracted with ethyl acetate (3×10 ml)
3. dry with materialThe combined organics were dried over sodium sulfate
4. concentrationconcentrated to a residue which
5. customwas purified by reverse phase chromatography on a preparative LC/UV/MS system
6. washCompounds were eluted from the HPLC column (Maccel 120-10-C18 SH 10 μm 20 mmID×50 mm) at 88 ml/min with 5-95 acetonitrile/water gradient