참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,5-Dichloro-2-cyanopyridine | HCID 2769699 | — |
| 반응물 | 1-(4-Ethynylphenyl)ethan-1-one | HCID 5123626 | — |
| 반응물 | triethylamine N,N-dimethylformamide | HCID 22056947 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | HCID 66874911 | HCID 66874911 | — |
반응 단계
To a solution of 1-(4-ethynylphenyl)ethanone (commercially available) (1 eq) 3,5-dichloropicolinonitrile (1 eq), dichlorobis(triphenylphosphine)-palladium (II) (20 mol %), copper iodide (10 mol %) and DMF: Triethylamine (10:1) (0.13 M) was stirred at ambient temperature overnight. The reaction mixture was then diluted with ethyl acetate and sodium bi-carbonate solution. The two phases were separated, and the aqueous phase was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, and concentrated en vaccuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-100% ethyl acetate in hexane and 5-((4-acetylphenyl)ethynyl)-3-chloropicolinonitrile was isolated as a yellow solid
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08466167B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_06 |
|---|
| ORD ID | ord-5721af2c721b467785e05c058ef338f0 |
|---|
| 출처 메모 | uspto-grants-2013_06 |
|---|
