HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19708608, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Bromo-4-methyl-2-pyridinecarbonitrile | HCID 19708610 | — |
| Reactant | HCID 178481859 | HCID 178481859 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19708608 | HCID 19708608 | 74.4% |
Reaction Steps
7.6 g 2-bromo-6-cyano-4-methylpyridine, 9 g 1-methyl-3-trifluoromethyl-5-hydroxypyrazole and 9.7 g potassium carbonate were mixed in 30 ml N,N-dimethylformamide and heated to reflux for 5 hours. After cooling, the reaction mixture was poured into 300 ml water and the aqueous layer extracted three times each with 100 ml ethyl acetate. The combined extracts were dried with anhydrous magnesium sulphate and the solvent removed in vacuo. Purification by silica gel column chromatography using hexane/ethyl acetate 7:3 afforded 8.1 g (50%) of the title compound as a pale brown solid of melting point 88° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05707932 |
| Source dataset | uspto-grants-1998_01 |
| ORD ID | ord-e17e0aa794fb42d38aeba9bf01cb32ad |
| Source note | uspto-grants-1998_01 |