Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-[(2-Methylbut-3-yn-2-yl)oxy]benzonitrile → Benzyl 2-[3-(4-cyanophenoxy)-3-methyl-1-butyn-1-yl]pyridine-5-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-[(2-Methylbut-3-yn-2-yl)oxy]benzonitrile | HCID 2779072 | — |
| 반응물 | HCID 19895696 | HCID 19895696 | — |
| 촉매 | Triphenylphosphine | HCID 11776 | — |
| 촉매 | Palladium Chloride | HCID 24290 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Diethylamine | HCID 8021 | — |
| 생성물 | Benzyl 2-[3-(4-cyanophenoxy)-3-methyl-1-butyn-1-yl]pyridine-5-carboxylate | HCID 19895702 | 74.9% |
반응 단계
12.2 g of benzyl 2-iodopyridine-5-carboxylate and 5.64 g of 4-(1,1-dimethyl-2-propynyloxy)benzonitrile were stirred with 32 mg of copper(I) iodide, 162 mg of triphenylphosphine and 180 mg of palladium(II) chloride in 280 ml of diethylamine at room temperature for 7 days under a nitrogen atmosphere. The mixture was evaporated and the residue was taken up in ethyl acetate and water. The organic phase was separated, dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:4) for the elution. There were obtained 9.04 g of benzyl 2-[3-(4-cyanophenoxy)-3-methyl-1-butyn-1-yl]pyridine-5-carboxylate which was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04971982 |
| 출처 데이터셋 | uspto-grants-1990_11 |
| ORD ID | ord-8614dd0ab5c04322b44c419a256b1f64 |
| 출처 메모 | uspto-grants-1990_11 |