反应详情

A 3 M DCM solution of bromoformonitrile (0.2 mL, 0.6 mmol) (commercially available from Aldrich) was mixed with imidazole (0.157 g, 2.3 mmol) (commercially available from Aldrich) in 10 mL DCM. The mixture was heated and maintained to reflux for 30 minutes in a round bottom flask. After the DCM was removed under a reduced pressure, isoquinoline-6-carbohydrazide (0.1 g, 0.53 mmol) suspended in 50 mL THF was added into the flask. The mixture was heated and maintained at reflux for 3 hours. After removing the THF, the remaining residue was mixed with 10 mL water and filtered. After washing with water and air drying, a white solid was obtained as the desired product (0.107 g, 96%) LCMS (API-ES) m/z (%): 213.0 (100%, M++H).

1. temperatureThe mixture was heated
2. temperaturemaintained
3. temperatureto reflux for 30 minutes in a round bottom flask
4. additionwas added into the flask
5. temperatureThe mixture was heated
6. temperaturemaintained
7. temperatureat reflux for 3 hours
8. customAfter removing the THF
9. additionthe remaining residue was mixed with 10 mL water
10. filtrationfiltered
11. washAfter washing with water and air
12. customdrying