HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → N-(6-{[({[3-(dimethylamino)phenyl](1-methyl-1H-tetrazol-5-yl)methylene}amino)oxy]methyl}pyridin-2-yl)-2,2-difluoro-2-phenoxyacetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 6-{[({[3-(dimethylamino)phenyl](1-methyl-1H-tetrazol-5-yl)methylene}amino)oxy]methyl}pyridin-2-amine | HCID 86653151 | — |
| Reactant | 2,2-Difluoro-2-phenoxyacetyl chloride | HCID 86656404 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | N-(6-{[({[3-(dimethylamino)phenyl](1-methyl-1H-tetrazol-5-yl)methylene}amino)oxy]methyl}pyridin-2-yl)-2,2-difluoro-2-phenoxyacetamide | HCID 86656403 | 88% |
Reaction Steps
To a stirred solution of 6-{[({[3-(dimethylamino)phenyl](1-methyl-1H-tetrazol-5-yl)methylene}amino)oxy]methyl}pyridin-2-amine (90 mg, 0.26 mmol) in dry 1,4-dioxane (10 mL) were added pyridine (31 μL, 0.38 mmol) and 2,2-difluoro-2-phenoxyacetyl chloride (105 mg, 0.51 mmol). The reaction mixture was stirred at room temperature for 25 h, then poured into aq. NaHCO3 (10 g/L, 30 mL). After extraction with ethyl acetate (50 mL), the organic layer was dried (MgSO4) and concentrated in vacuo. Purification on silica gel afforded N-(6-{[({[3-(dimethylamino)phenyl](1-methyl-1H-tetrazol-5-yl)methylene}amino)oxy]methyl}pyridin-2-yl)-2,2-difluoro-2-phenoxyacetamide as an oil [123 mg, yield 88%; HPLC/MS:m/z=523 (M+H); log P(HCOOH)=4.14].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08492388B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-57f5d1f4ef4f46cea0ad6adca34f77e9 |
| Source note | uspto-grants-2013_07 |