Reaction equation
[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([F:11])=[CH:6][C:3]=1[C:4]#N.S(=O)(=O)(O)[OH:13].[OH2:17]>>[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([F:11])=[CH:6][C:3]=1[C:4]([OH:13])=[O:17]Participants
4
Procedure
2.10 g of the 2-chloro-4,5-difluorobenzonitrile obtained as above and 12 ml of 60% sulfuric acid were reacted under reflux for 10 hour. After cooling, the mixture was diluted with 20 ml of water and then extracted with chloroform (10ml×2 times). The extract was washed with water and dried, and then the the solvent was distilled off to obtain 2.20 g (yield: 94.8%) of 2 -chloro-4,5-difluorobenzoic acid. Melting point: 103°-105° C.
Workup
- customwere reacted
- temperatureunder reflux for 10 hour
- temperatureAfter cooling
- extractionextracted with chloroform (10ml×2 times)
- washThe extract was washed with water
- customdried
- distillationthe the solvent was distilled off
Sources & evidence
- ORD record
- ord-5da1a7f6fa2b47cf9e44a6753f2fa40f
- Source dataset
- uspto-grants-1994_07
- Patent number
- US05332851
Linked notes
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