関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Picolinic acid | HCID 1018 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | Benzene, 1-iodo-3-methoxy- | HCID 69839 | — |
| 反応物 | 4-(2-Aminopyridin-3-yl)phenol | HCID 66748477 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3-(4-(3-Methoxyphenoxy)phenyl)pyridin-2-amine | HCID 66748860 | 44.5% |
反応手順
Copper(I) iodide (102 mg) was added to a mixture of picolinic acid (66.1 mg), 4-(2-aminopyridin-3-yl)phenol (500 mg), tripotassium phosphate (1710 mg), 1-iodo-3-methoxybenzene (754 mg) and DMSO (8 mL). The mixture was stirred at 120° C. under nitrogen for 6 hr. The insoluble material was removed by silica-filtration with EtOAc, and the filtrate was extracted with EtOAc. The organic layer was separated, washed with water and brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (NH silica gel, eluted with EtOAc in hexane) to give the title compound (349 mg) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08575154B2 |
|---|
| 出典データセット | uspto-grants-2013_11 |
|---|
| ORD ID | ord-f8648584582542e595713a83f68fbf16 |
|---|
| 出典メモ | uspto-grants-2013_11 |
|---|
