Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Dichloroacetyl chloride | HCID 6593 | — |
| Reactant | 5-Amino-1-(2,3,5,6-tetrafluoro-4-trifluoromethylphenyl)pyrazole | HCID 13933709 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13933710 | HCID 13933710 | 85.4% |
Reaction Steps
1.8 ml (0.022 mol) of anhydrous pyridine and 2.1 ml (0.021 mol) of 98 percent pure dichloroacetyl chloride are added in succession to a solution of 6 g (0.02 mol) of 5-amino-1-(2,3,5,6-tetrafluoro-4-trifluoromethylphenyl)-pyrazole in 35 ml of anhydrous acetonitrile. The temperature rises to 35° C. The mixture is subsequently stirred for four hours and then poured onto 150 ml of water. The oily precipitate is taken up in 50 ml of methylene chloride, the aqueous phase is separated off and the organic phase is washed with dilute hydrochloric acid, saturated sodium bicarbonate solution and saturated sodium chloride solution in succession, dried over magnesium sulphate and freed from the solvent in vacuo. 7.0 g (85% of theory) of 5-dichloroacetamido-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole of melting point 112° C.-114° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04787930 |
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| Source dataset | uspto-grants-1988_11 |
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| ORD ID | ord-f2dabe2dec8240259bea1f16aa4c4489 |
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| Source note | uspto-grants-1988_11 |
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