反应详情

Under argon, 0.80 g (2.61 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamidine from Example 6A, 0.51 g (2.86 mmol) of sodium (E)-2-cyano-2-[(methoxycarbonyl)(methyl)amino]ethenolate from Example 10A and 0.53 g (0.73 ml, 5.23 mmol) of triethylamine are added to 50 ml of toluene. The mixture is heated under reflux for 9 hours. It is then cooled to RT again and is mixed and extracted with dichloromethane and water. The organic phase is dried over magnesium sulphate, filtered and concentrated in vacuo in a rotary evaporator. The residue is mixed with 5 ml of diethyl ether and crystallizes therewith. The crystals are filtered off with suction, dried and purified by preparative RP-HPLC.

1. temperatureThe mixture is heated
2. temperatureunder reflux for 9 hours
3. additionis mixed
4. extractionextracted with dichloromethane and water
5. dry with materialThe organic phase is dried over magnesium sulphate
6. filtrationfiltered
7. concentrationconcentrated in vacuo in a rotary evaporator
8. additionThe residue is mixed with 5 ml of diethyl ether
9. customcrystallizes
10. filtrationThe crystals are filtered off with suction
11. customdried
12. custompurified by preparative RP-HPLC