反应详情

温度

100 °C

2-Ethoxy-N-(5-iodo-4-methyl-2-propylimidazol-1-yl)benzamide from Example 1a (0.5 g, 1.2 mmol) and copper(I) cyanide (0.7 g, 7.5 mmol) are introduced into 10 ml of pyridine and heated at 100° C. for three hours. The reaction mixture is cooled to room temperature, 50 ml of dichloromethane are added, and the solid is removed by filtration. The filtrate is washed three times with 50 ml of water each time, and the organic phase is re-extracted with 50 ml of dichloromethane. The combined organic phase is dried with sodium sulphate and concentrated. To remove the remaining pyridine, the residue is taken up in 50 ml of dichloromethane and washed six times with 100 ml of water each time. The organic phase is dried with sodium sulphate and concentrated in a rotary evaporator. The residue is finally mixed with 100 ml of toluene and concentrated.

1. temperatureThe reaction mixture is cooled to room temperature
2. customthe solid is removed by filtration
3. washThe filtrate is washed three times with 50 ml of water each time
4. extractionthe organic phase is re-extracted with 50 ml of dichloromethane
5. dry with materialThe combined organic phase is dried with sodium sulphate
6. concentrationconcentrated
7. customTo remove the remaining pyridine
8. washwashed six times with 100 ml of water each time
9. dry with materialThe organic phase is dried with sodium sulphate
10. concentrationconcentrated in a rotary evaporator
11. additionThe residue is finally mixed with 100 ml of toluene
12. concentrationconcentrated