Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Methylbut-1-yne → 4-Methoxy-1-(3-methylbut-1-ynyl)-2-nitrobenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Methylbut-1-yne | HCID 69019 | — |
| 반응물 | 4-Iodo-3-nitroanisole | HCID 292659 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 4-Methoxy-1-(3-methylbut-1-ynyl)-2-nitrobenzene | HCID 59762351 | — |
반응 단계
To a solution of 1-iodo-4-methoxy-2-nitrobenzene (Aldrich, 10 g, 35.8 mmol) in Et3N (60 ml) and DMF (6 ml) was added CuI (34 mg, 0.18 mmol), Pd(PPh3)2Cl2 (126 mg, 0.18 mmol), and 3-methyl-1-butyne (5.0 ml, 73.5 mmol). The mixture was stirred at room temperature for 16 h and was concentrated. The resulting mixture was diluted with EtOAc, washed with H2O, brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→15% EtOAc-hexanes) to yield the title compound as a brown oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524917B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-b7a226b1c835495eaf8a21b6a00f0eb4 |
| 출처 메모 | uspto-grants-2013_09 |