HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic anhydride → 3-[5-(3,4-Dimethoxy-5-nitro-phenyl)-pyrazol-1-yl]-2-trifluoromethyl-pyridine 1-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 67036978 | HCID 67036978 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-[5-(3,4-Dimethoxy-5-nitro-phenyl)-pyrazol-1-yl]-2-trifluoromethyl-pyridine 1-oxide | HCID 67036890 | — |
Reaction Steps
To a solution of 3-[5-(3,4-dimethoxy-5-nitro-phenyl)-pyrazol-1-yl]-2-trifluoromethyl-pyridine (0.50 g, 1.27 mmol) in dichloromethane (10 mL) cooled in an ice-water bath was added urea-hydrogen peroxide complex (0.26 g, 2.76 mmol) in one portion followed by trifluoroacetic anhydride (0.53 g, 2.52 mmol) dropwise. The resulting mixture was allowed to stir at room temperature overnight and then the insoluble material was filtered off. The filtrate was washed with water and brine, then dried over anhydrous sodium sulphate, filtered and evaporated to leave an off-white solid. Recrystallisation from ethanol afforded 3-[5-(3,4-dimethoxy-5-nitro-phenyl)-pyrazol-1-yl]-2-trifluoromethyl-pyridine 1-oxide, 0.34 g (65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08907099B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-21170d0ae59647229cac919eb1f769b6 |
| Source note | uspto-grants-2014_12 |