反应详情

温度

100 °C

A solution of 4-hydroxy-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid (2.0 g, 7.4 mmol) in phosphorous oxychloride (15 mL, 63 mmol) was heated and stirred at 100° C. for 3 hours. After the solution was cooled to room temperature, the solvent was evaporated under reduced pressure. The residue was dissolved in tetrahydrofuran (50 mL). To the solution, a solution of N-methylaniline (1.0 mL, 9.2 mmol) and triethylamine (5.2 mL, 37 mmol) in tetrahydrofuran (10 mL) was added at 0° C. After the mixture was stirred at room temperature for 1.5 hours, the reaction solvent was evaporated under reduced pressure. Purification of the residue thus obtained by silica gel chromatography (chloroform:methanol=50:1 to 20:1) gave the title compound (2.14 g, 76% yield).

1. temperatureAfter the solution was cooled to room temperature
2. customthe solvent was evaporated under reduced pressure
3. dissolutionThe residue was dissolved in tetrahydrofuran (50 mL)
4. stirringAfter the mixture was stirred at room temperature for 1.5 hours
5. customthe reaction solvent was evaporated under reduced pressure
6. customPurification of the residue
7. customthus obtained by silica gel chromatography (chloroform:methanol=50:1 to 20:1)