反应详情

温度

0 °C

30.5 g (87.0 mmol) of 2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4,5,6-pyrimidinetriamine trihydrochloride from Example 8A are dissolved in 30 ml of pyridine. The resulting solution is cooled to 0° C. 8.22 g (87.0 mmol) of methyl chloroformate are added, and the mixture is stirred at 0° C. for a further 2 hours. It is subsequently allowed to warm to room temperature and is stirred for a further 12 hours. After concentration in vacuo, the residue is washed with water and dried. Further purification is effected by stirring in 300 ml of boiling diethyl ether. The precipitated product is filtered off with suction and dried in vacuo.

1. temperatureto warm to room temperature
2. stirringis stirred for a further 12 hours
3. concentrationAfter concentration in vacuo
4. washthe residue is washed with water
5. customdried
6. customFurther purification
7. stirringby stirring in 300 ml of boiling diethyl ether
8. filtrationThe precipitated product is filtered off with suction
9. customdried in vacuo