Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Fluoro-3-iodobenzene → 1-[3-(3-Fluorophenyl)-2-propynyl]4-methylpiperidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Fluoro-3-iodobenzene | HCID 70725 | — |
| 반응물 | 4-Methyl-1-(prop-2-yn-1-yl)piperidine | HCID 11355509 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 촉매 | Tri(o-toluoyl)phosphine | HCID 19696886 | — |
| 용매 | Diethylamine | HCID 8021 | — |
| 생성물 | 1-[3-(3-Fluorophenyl)-2-propynyl]4-methylpiperidine | HCID 9899438 | 56.2% |
반응 단계
A mixture of 3-fluoroiodobenzene (8.88 g), 4-methyl-1-(2-propynyl)piperidine (6.80 g), palladium acetate (0.045 g), tri-o-toloylphosphine (0.24 g) and copper(I) iodide (0.1 g) in dry diethylamine (50 ml) was heated under reflux for 5 hours. The solvent was removed under reduced pressure and the residue was taken up in diethyl ether and washed with water. The organic phase was dried over magnesium sulfate and the solvent was removed under reduced pressure. Distillation of the residue under reduced pressure gave an oil (5.20 g) of boiling point 105° C./0.07 mm Hg.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07084158B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-407eb598551c4c3b88f8f45387ed5837 |
| 출처 메모 | uspto-grants-2006_08 |