Phosphorus oxychloride → HCID 57799845, compound
Reaction equation
[CH3:1][O:2][C:3]1[C:4]([CH3:21])=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][C:7]([NH:14][C:15]1[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=1)=[CH:6]2.O=P(Cl)(Cl)[Cl:24]>>[Cl:24][C:9]1[C:10]2[C:5](=[C:4]([CH3:21])[C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[C:7]([NH:14][C:15]2[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=2)[N:8]=1Participants
3
Conditions
- Temperature
- 150 °C
Procedure
A 10˜20 mL process vial was charged with 500 mg 6-Methoxy-5-methyl-3-(5-methyl-1H-pyrazol-3-ylamino)-2H-isoquinolin-1-one in 15 mL POCl3. The vial was heated at 150° C. for 30 min under microwave irradiation. After cooling, POCl3 was removed under reduced pressure. MeOH was carefully added to the residue during which the precipitate was formed. The solid was collected as crude product for the next reaction.