Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Methylbut-1-yne → 2-Chloro-5-(3-methylbut-1-ynyl)pyridin-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Methylbut-1-yne | HCID 69019 | — |
| 반응물 | 2-Chloro-5-iodopyridin-4-amine | HCID 45480366 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 2-Chloro-5-(3-methylbut-1-ynyl)pyridin-4-amine | HCID 58025064 | — |
반응 단계
To a solution of 2-chloro-5-iodopyridin-4-amine (Compound 11, 2.55 g, 10.0 mmol) in Et3N (35 ml) was added Pd(PPh3)2Cl2 (70 mg, 0.10 mmol), CuI (19 mg, 0.10 mmol), and 3-methyl-1-butyne (1.2 ml, 12 mmol). The reaction was stirred at room temperature for 20 h and was quenched with H2O, extracted with EtOAc (Δ2). The combined organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes) to yield the title compound as an off-white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536339B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-c536abf1d78f45489380ea426fc5482d |
| 출처 메모 | uspto-grants-2013_09 |