Thionyl Chloride → HCID 11694729, compound
Reaction equation
S(Cl)([Cl:3])=O.[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:13]2[O:14][C:15]([CH3:20])=[C:16]([CH3:19])[N+:17]=2[O-])[CH:10]=[CH:11][CH:12]=1>>[ClH:3].[Cl:3][CH2:19][C:16]1[N:17]=[C:13]([C:9]2[CH:10]=[CH:11][CH:12]=[C:7]([O:6][CH3:5])[CH:8]=2)[O:14][C:15]=1[CH3:20]Participants
3
Procedure
The entire toluenic solution from Example 1 (420 ml) was admixed at 60° C. dropwise with 54.2 g (0.456 mol) of thionyl chloride and stirred at <60° C. for up to 22 h. Subsequently, the mixture was concentrated by distilling off 229 ml. The suspension was cooled to <20° C., and the product was isolated by filtration with suction, washed 3 times with 20 ml each time of toluene and dried at elevated temperature under reduced pressure.
Workup
- concentrationSubsequently, the mixture was concentrated
- distillationby distilling off 229 ml
- temperatureThe suspension was cooled to <20° C.
- customthe product was isolated by filtration with suction
- wash