5-CHLORO-1-METHYL-3-(TRIFLUOROMETHYL)PYRAZOLE-4-CARBOXALDEHYDE synthesis
- Product Name:5-CHLORO-1-METHYL-3-(TRIFLUOROMETHYL)PYRAZOLE-4-CARBOXALDEHYDE
- CAS Number:128455-62-9
- Molecular formula:C6H4ClF3N2O
- Molecular Weight:212.56
356759-12-1
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Yield:-
Reaction Conditions:
with sodium hydroxide;trichlorophosphate in N,N-dimethyl-formamide
Steps:
1 Synthesis of 1-methyl-3-trifluoromethyl-5-chloropyrazole-4-carboxylic acid
1) 21.35 g of phosphorus oxychloride was dropwise added to 4.72 g of DMF at 10° C. or lower. After the temperature of the reaction solution was returned to room temperature, the reaction mixture was stirred for 1 hour, and 10.71 g of 1-methyl-3-trifluoromethyl-5-pyrazolone was added thereto. The resulting mixture was heated up to 110° C., and stirred for 7 hours. After having been left to be at 70° C. the reaction mixture was poured into ice water. After pH of the mixture was made to be about 4 with an aqueous solution of sodium hydroxide added thereto, and precipitated crystals were taken out through filtration and dried to obtain 10.55 g of 1-methyl-3-trifluoromethyl-5-chloropyrazole-4-carbaldehyde.
References:
Nissan Chemical Industries, Ltd. US6063734, 2000, A