Trifluoroacetic acid → HCID 21498238, compound
Reaction equation
[NH:1]([C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([CH3:13])=[CH:5][N:4]=1)[NH2:2].[F:14][C:15]([F:20])([F:19])[C:16](O)=O>>[F:14][C:15]([F:20])([F:19])[C:16]1[N:4]2[CH:5]=[C:6]([CH3:13])[C:7]3[C:12]([C:3]2=[N:1][N:2]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3Participants
3
Procedure
1-Hydrazino-4-methylisoquinoline (5.0 g.) and trifluoroacetic acid (70 ml.)were heated at reflux for three hours. After removal of the excess trifluoroacetic acid, the residue was dissolved in chloroform and extracted with sodium carbonate solution. The organic layer was dried and concentrated and the residue was recrystallized from a cyclohexane-benzene(70/30) mixture to provide the product in a yield of 65%, m.p. 162°-164°C.
Workup
- temperature)were heated
- temperatureat reflux for three hours
- customAfter removal of the excess trifluoroacetic acid
- dissolutionthe residue was dissolved in chloroform
- extractionextracted with sodium carbonate solution
- customThe organic layer was dried
- concentrationconcentrated
- customthe residue was recrystallized from a cyclohexane-benzene(70/30) mixture
- customto provide the product in a yield of 65%, m.p. 162°-164°C.
Sources & evidence
- ORD record
- ord-540a9130aa6643e5bf19b419f1c8ba0f
- Source dataset
- uspto-grants-1976_11
- Patent number
- US03992539
Reaction notes
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