Carbon Dioxide → 2,6-Dichloro-3,5-difluorophenol
Reaction equation
[Cl:1][C:2]1[C:3]([F:14])=[C:4]([C:8]([F:13])=[C:9]([Cl:12])[C:10]=1[OH:11])C(O)=O.CN(C)C=O.C(=O)=O.C1(C)C=CC=CC=1>O>[Cl:1][C:2]1[C:3]([F:14])=[CH:4][C:8]([F:13])=[C:9]([Cl:12])[C:10]=1[OH:11]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
50 g of 3,5-dichloro-2,6-difluoro-4-hydroxy-benzoic acid and 10 ml of dimethylformamide are mixed and heated. At 105°-130° C., carbon dioxide evolves, and the reaction is allowed to run to completion at this temperature. 200 ml of toluene and then 80 ml of water are subsequently stirred into the mixture, the phases are separated, and the organic phase is dried and subsequently distilled. 34 g product of boiling point 87°-8° C. are obtained; nD20 : 1.5310.
Workup
- temperatureheated
- customAt 105°-130° C.
- customthe phases are separated
- customthe organic phase is dried
- distillationsubsequently distilled
Sources & evidence
- ORD record
- ord-df4fc3a3e96e418bb671f72a22ec65c8
- Source dataset
- uspto-grants-1993_11
- Patent number
- US05260474
Reaction notes
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