反应详情

温度

80 °C

In a round-bottomed flask, 2-bromo-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid isopropylamide (300 mg, 0.73 mmol) and 5-(tert-butyl-dimethyl-silanyloxymethyl)-1-methyl-3-tributylstannanyl-1H-indazole (Example 273, 665 mg, 0.82 mmol) were dissolved in DMF (4.8 ml). The reaction mixture was evacuated and backfilled with argon then tetrakis(triphenylphosphine)palladium (0) (42 mg, 0.036 mmol) and copper (I) iodide (28 mg, 0.147 mmol) were added. The reaction mixture was stirred at 80° C. overnight then cooled to room temperature, quenched with water and diluted with petroleum ether. The resulting suspension was filtered and the solids washed with water, petroleum ether and a minimal amount of diethyl ether then dried under high vacuum to afford 426 mg (92%) of 2-[5-(tert-butyldimethyl-silanyloxymethyl)-1-methyl-1H-indazol-3-yl]-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid isopropylamide as a brown powder.

1. customThe reaction mixture was evacuated
2. temperaturethen cooled to room temperature
3. customquenched with water
4. additiondiluted with petroleum ether
5. filtrationThe resulting suspension was filtered
6. washthe solids washed with water, petroleum ether
7. dry with materiala minimal amount of diethyl ether then dried under high vacuum