참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetamide | HCID 178 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-Chloro-4-((6-nitropyridin-3-yl)oxy)pyridine | HCID 59322779 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 촉매 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | N-(4-((6-nitropyridin-3-yl)oxy)pyridin-2-yl)acetamide | HCID 90409856 | 68% |
반응 단계
A degassed solution of Example A1 (2.0 g, 7.95 mmol) in dioxane (30 mL) added treated with acetamide (1.878 g, 31.8 mmol), Cs2CO3 (2.59 g, 7.95 mmol), X-Phos (0.189 g, 0.397 mmol), and Pd2(dba)3 (0.364 g, 0.397 mmol) and heated at 80° C. for 16 h. The mixture was cooled to RT, treated with EtOAc, the solids removed via filtration through diatomaceous earth and rinsed well with EtOAc. The filtrate was washed with water, then brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford N-(4-((6-nitropyridin-3-yl)oxy)pyridin-2-yl)acetamide (1.48 g, 68%). MS (ESI) m/z: 275.1 (M+H+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09309224B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_04 |
|---|
| ORD ID | ord-b3c4a19b1b1e40a3bb8d496342721504 |
|---|
| 출처 메모 | uspto-grants-2016_04 |
|---|
