HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86585634, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Chloro(chlorosulfanyl)difluoromethane | HCID 12621923 | — |
| Reactant | HCID 178510263 | HCID 178510263 | — |
| Product | HCID 86585634 | HCID 86585634 | 71% |
Reaction Steps
To the solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-hydroxypyrazole (12.0 g, 37.3 mmol.) and pyridine (3.25 g, 41.0 mmol) in dichloromethane at −50-−60 C. was added chlorodifluoromethanesulfenyl chloride (8.1 g, 46.6 mmol). The resulting solution was gradually warmed up to room temperature. After 20 hr, the organic layer was washed five times with water. It was then washed with brine and dried (Na2SO4) to provide an oil. Upon chromatographic purification of the oil , a total of 11.6 g (26.4 mmol., 71% yield) of the desired product with 97% HPLC puriety was isolated. F-NMR: −30.05 ppm (CCIF2), −63.80 ppm (ArCF3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06569886B2 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-60e0e5e3135b44b29cb26a870f4454ca |
| Source note | uspto-grants-2003_05 |