Water → HCID 19754735, compound
Reaction equation
[F-:1].[K+].Cl[C:4]1[N:8]([CH3:9])[N:7]=[C:6]([CH:10]([F:12])[F:11])[C:5]=1[CH:13]=[O:14].O>CN(C)C=O>[F:1][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([CH:10]([F:12])[F:11])[C:5]=1[CH:13]=[O:14]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 150 °C
Procedure
To 96.3 g (1660 mmol) of spray-dried potassium fluoride, was added a solution of 129.2 g (664 mmol) of 5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde in 1000 ml of dimethylformamide. The resulting reaction mixture was stirred at 150° C. for 3 hours. The reaction mixture was cooled to room temperature and to it was added 4 L of water. The aqueous phase was extracted with ethyl acetate. The combined organic phase were washed with brine, dried over sodium sulphate and evaporated under vacuum to give the expected product.
Workup
- customThe resulting reaction mixture
- temperatureThe reaction mixture was cooled to room temperature and to it
- extractionThe aqueous phase was extracted with ethyl acetate
- washThe combined organic phase were washed with brine
- dry with materialdried over sodium sulphate
- customevaporated under vacuum
Sources & evidence
- ORD record
- ord-24315fa1c22c44f08ac75a325c1d6fb4
- Source dataset
- uspto-grants-2014_07
- Patent number
- US08772266B2
Reaction notes
Loading…