HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 5-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Cyanoacetyl chloride | HCID 11051594 | — |
| Reactant | 5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole | HCID 13557109 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 5-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole | HCID 13985067 | 80% |
Reaction Steps
22.5 g (0.076 mol) of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole and 8 g (0.1 mol) of pyridine are taken in 200 ml of acetonitrile, and 13.2 g (0.128 mol) of cyanoacetyl chloride are added dropwise at 20°-25° C., while stirring and cooling. The reaction mixture is stirred at room temperature for a further two hours and then poured into water. After extraction with methylene chloride and drying of the organic phase over sodium sulphate, the solvent is distilled off in vacuo. The crystalline residue is stirred with a mixture of ligroin and diisopropyl ether and filtered off with suction. 22 g (80% of theory) of 5-cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 169°-175° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04814001 |
| Source dataset | uspto-grants-1989_03 |
| ORD ID | ord-766122a87d3147c59c59249c7b8aa355 |
| Source note | uspto-grants-1989_03 |