Trifluoroacetic acid → HCID 23149183, compound
Reaction equation
[Cl:1][C:2]([Cl:19])([F:18])[S:3][C:4]1[CH:5]=[N:6][N:7](CC2C=CC(OC)=CC=2)[CH:8]=1.FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+]>>[Cl:1][C:2]([Cl:19])([F:18])[S:3][C:4]1[CH:5]=[N:6][NH:7][CH:8]=1Participants
4
Conditions
- Temperature
- 65 °C
Procedure
1.04 g of 4-{[dichlorofluoromethyl]thio}-1-(4-methoxybenzyl)-1H-pyrazole was dissolved to 6 ml of trifluoroacetic acid, followed by stirring at 65° C. for 3 hours. After the reaction mixture was cooled to room temperature, it was added to saturated aqueous solution of sodium hydrogen carbonate. The mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.19 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole.
Workup
- temperatureAfter the reaction mixture was cooled to room temperature
- extractionThe mixture was extracted with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure
Sources & evidence
- ORD record
- ord-131e44626a8d4a1390e459e58d5a8591
- Source dataset
- uspto-grants-2009_06
- Patent number
- US07541374B2
Reaction notes
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