反应 #66093

反应方程式

3-bromo-1H-pyrazolo[3,4-c]-pyridine

1,4-diazabicyclo[3.2.2]nonane

triethylamine

N,N-dimethylformamide

→

3-(1,4,Diazabicyclo[3.2.2]non-4-ylcarbonyl)-1H-pyrazolo[3,4-c]pyridine

反应条件

后处理

1. 1
   workup.ADDITIONare successively introduced into a 50 ml reactor
2. 2
   其他The mixture is then purged with carbon monoxide
3. 3
   workup.ADDITIONThe reaction medium is poured into 100 ml of water
4. 4
   萃取the aqueous phase is extracted with chloroform
5. 5
   其他After drying the organic phases, they
6. 6
   其他are dried
7. 7
   过滤filtered
8. 8
   浓缩concentrated under reduced pressure
9. 9
   其他The residue is purified by chromatography on a column of silica gel
10. 10
    洗涤eluting with a mixture of chloroform, methanol and aqueous ammonia in 90/10/1 proportions

实验过程

1 g (5 mmol) of 3-bromo-1H-pyrazolo[3,4-c]-pyridine, 0.53 g (0.75 mmol) of bis(triphenylphosphino)dichloropalladium, 1.9 g (15.1 mmol) of 1,4-diazabicyclo[3.2.2]nonane and 3.5 ml (25 mmol) of triethylamine dissolved in 15 ml of N,N-dimethylformamide are successively introduced into a 50 ml reactor. The mixture is then purged with carbon monoxide and heated at 110° C. for 20 hours. The reaction medium is poured into 100 ml of water and the aqueous phase is extracted with chloroform. After drying the organic phases, they are dried, filtered and concentrated under reduced pressure. The residue is purified by chromatography on a column of silica gel, eluting with a mixture of chloroform, methanol and aqueous ammonia in 90/10/1 proportions.

来源