反应详情

温度

170 °C

0.2 g (1.05 mmol) of copper iodide, 0.6 g (2.10 mmol) of 5-fluoro-1-[(3-fluorophenyl)-methyl]-1H-indole-2-carboxamide, prepared according to the protocol described in step 1.2, 0.4 g (2.31 mmol) of 2-amino-4-bromopyridine, 1.16 g (8.40 mmol) of potassium carbonate and 15 mL of anhydrous dioxane are placed in a 10 mL pressure tube specific for microwave reactors. The suspension is degassed for a few minutes and 0.14 mL (1.15 mmol) of trans-1,2-cyclohexanediamine is then added. The tube is then sealed and heated in the microwave reactor at 170° C. for two 1-hour cycles, After this time, the suspension cooled to room temperature is poured into 50 mL of water and then extracted with 2×75 mL of dichlororomethane. The combined organic phases are dried over magnesium sulfate and concentrated under reduced pressure. The crude reaction product is then purified by chromatography on a column of silica gel, eluting with a mixture of dichloromethane and methanol. 0.425 g of the expected product is thus obtained in the form of a beige-coloured solid.

1. customare placed in a 10 mL pressure tube
2. customThe suspension is degassed for a few minutes
3. customThe tube is then sealed
4. temperatureAfter this time, the suspension cooled to room temperature
5. extractionextracted with 2×75 mL of dichlororomethane
6. dry with materialThe combined organic phases are dried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe crude reaction product
9. customis then purified by chromatography on a column of silica gel
10. washeluting with a mixture of dichloromethane and methanol