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-hydroxybenzoic acid and 10 ml of dimethylformamide are mixed, and the mixture is heated. Carbon dioxide is evolved at 105°-130° C., and the mixture is allowed to react at this temperature until the reaction is complete. After this, 200 ml of toluene and then 80 ml of water are stirred in, the phases are separated, and the organic phase is dried and then distilled. This gives 34 g of the product having a boiling point of 87°-88° C. and a refractive index of [n]D20 : 1.5310.
Workup
- temperaturethe mixture is heated
- customis evolved at 105°-130° C.
- customto react at this temperature until the reaction
- customare separated
- customthe organic phase is dried
- distillationdistilled
Sources & evidence
- ORD record
- ord-d60ebe012c544bc693d0978ccf5ab60d
- Source dataset
- uspto-grants-1992_11
- Patent number
- US05166392
Reaction notes
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