反应详情

The starting material 4-chloro-7-methoxycinnoline hydrochloride was obtained by heating a solution of 4-hydroxy-7-methoxycinnoline (352 mg, 2 mmol), (prepared as described in J. Chem. Soc. 1955, 2100), in thionyl chloride (3.5 ml) containing DMF (20 μl) at reflux, for 1 hour. After removing excess thionyl chloride by evaporation and azeotroping with toluene. The residue was triturated with ether, filtered off and washed with ether to give 4-chloro-7-methoxycinnoline hydrochloride as a yellow solid (450 mg, 97%).

1. temperatureat reflux, for 1 hour
2. customAfter removing excess thionyl chloride
3. customby evaporation
4. customazeotroping with toluene
5. customThe residue was triturated with ether
6. filtrationfiltered off
7. washwashed with ether