反应详情

温度

135 °C

To a stirred slurry of 1,7-dichloro-5H-pyrido[4,3-b]indole-4-carbonitrile (16 g, 61 mmol) in dioxane (122 mL) was added dicyclopropylmethanamine (17 g, 153 mmol). The reaction mixture was heated to 135° C. for 1 d, cooled to room temperature, and concentrated. The residue was diluted with EtOAc and water. The aqueous layer was extracted with EtOAc (×3). The combined organics were washed with brine, dried (sodium sulfate), concentrated, and purified by flash chromatography to give the title compound. LRMS (APCI) calc'd for (C19H17ClN4) [M+H]+, 337.1. found 337.1.

1. temperaturecooled to room temperature
2. concentrationconcentrated
3. additionThe residue was diluted with EtOAc and water
4. extractionThe aqueous layer was extracted with EtOAc (×3)
5. washThe combined organics were washed with brine
6. dry with materialdried (sodium sulfate)
7. concentrationconcentrated
8. custompurified by flash chromatography