Water → HCID 21226441, compound
Reaction equation
Br[CH2:2][C:3]1[CH:4]=[C:5]([C:10]2[C:14]([Cl:15])=[C:13]([O:16][CH:17]([F:19])[F:18])[N:12]([CH3:20])[N:11]=2)[CH:6]=[CH:7][C:8]=1[Cl:9].[C:21]([O-:24])(=[O:23])[CH3:22].[Na+].O>CN(C)C=O>[C:21]([O:24][CH2:2][C:3]1[CH:4]=[C:5]([C:10]2[C:14]([Cl:15])=[C:13]([O:16][CH:17]([F:19])[F:18])[N:12]([CH3:20])[N:11]=2)[CH:6]=[CH:7][C:8]=1[Cl:9])(=[O:23])[CH3:22]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of 6.8 g (18 mmol) of 3-(3-bromomethyl-4-chlorophenyl)-4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazole and 1.5 g (18 mmol) of sodium acetate in 20 ml of dimethylformamide was stirred overnight and then stirred into 100 ml of cold water. The product was extracted from the aqueous phase using ethyl acetate. The ethyl acetate phase was dried over magneisum sulfate and concentrated. The crude product thus obtained was purified by silica gel chromatography (eluent: hexane/ethyl acetate=9:1). Yield: 4.7 g.
Workup
- extractionThe product was extracted from the aqueous phase
- dry with materialThe ethyl acetate phase was dried over magneisum sulfate
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-eaf2b77f50074646850fe9f17081f419
- Source dataset
- uspto-grants-1999_07
- Patent number
- US05928999
Reaction notes
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