Sulfuric Acid → HCID 23070158, compound
Reaction equation
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:12]3=[N:13][C:14](C#N)=[CH:15][CH:16]=[C:11]3[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.S(=O)(=O)(O)O.[C:24](=[O:27])([O-])[OH:25].[Na+]>O.C(O)(=O)C>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:12]3=[N:13][C:14]([C:24]([OH:25])=[O:27])=[CH:15][CH:16]=[C:11]3[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1Participants
6
Conditions
- Temperature
- 100 °C
Procedure
140 mg of 3-(3-fluorophenyl)-1H-pyrazolo[4,3-b]-pyridine-5-carbonitrile was added to a mixed solution of 1 mL water, 1 mL concentrated sulfuric acid and 1 mL glacial acetic acid, and heated under 100° C. for 3 hours. The reaction solution was added with 25 mL of ice-cooled water, neutralized with sodium hydrogen carbonate, and the precipitated crystals were collected by filtration. The crystals collected by filtration were washed with cold water, and dried under reduced pressure, to give 150 mg of a crude product of the title compound as a colorless powder.
Workup
- filtrationthe precipitated crystals were collected by filtration
- filtrationThe crystals collected by filtration
- washwere washed with cold water
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-2eadbb060ada48919d146a17c213ae40
- Source dataset
- uspto-grants-2008_09
- Patent number
- US07429609B2
Reaction notes
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