反应详情

温度

115 °C

A pressure tube containing copper (1) iodide (37.57 mg, 0.20 mmol), sodium iodide (591.42 mg, 3.95 mmol) and 4-(6-bromo-3-methyl-1H-indazol-1-yl)pyrimidin-2-amine (600 mg, 1.97 mmol) was flushed with nitrogen before the addition of 1,4-dioxane, DMF (3 ml each) and N,N′-dimethylethane-1,2-diamine (0.021 ml, 0.20 mmol). The vessel was sealed and stirred at 115° C. overnight. Reaction was cooled and added to ice water (15 ml) before extracting into DCM (2×20 mL). Combined organics were dried (Na2SO4), filtered and concentrated in vacuo. Crude material purified by column chromatography (Elution with 2% MeOH-DCM to 12% MeOH-DCM) to give the title compound: 1H NMR (500 MHz, DMSO) delta 7.02 (3H, dd, J=5.5, 3.1 Hz), 7.73-7.53 (2H, m), 8.25 (1H, d, J=5.5 Hz), 9.25 (1H, s); LC-MS: m/z=+351.90 (M+H)+. This compound of 79% purity LC-MS was used for the next step without further purification

1. customThe vessel was sealed
2. customReaction
3. temperaturewas cooled
4. extractionbefore extracting into DCM (2×20 mL)
5. dry with materialCombined organics were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customCrude material purified by column chromatography (Elution with 2% MeOH-DCM to 12% MeOH-DCM)