関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,10-Phenanthroline | HCID 1318 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1-Bromo-4-iodobenzene | HCID 11522 | — |
| 反応物 | 1-Ethyl-3-piperidinol | HCID 114524 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(4-Bromo-phenoxy)-1-ethyl-piperidine | HCID 67362850 | — |
反応手順
652 mg (2.00 mmol) caesium carbonate, 36 mg (0.20 mmol) 1,10-phenanthroline and 19 mg (0.10 mmol) CuI are added to a solution of 289 mg (1.00 mmol) 1-bromo-4-iodobenzene and 0.27 mL (2.00 mmol) N-ethyl-3-hydroxypiperidine in 1.0 mL toluene. The reaction mixture is stirred for 36 h at 110° C. and then combined with 10 mL water and 10 mL EtOAc. After filtration the aqueous phase is extracted with 10 mL EtOAc and the combined organic extracts are washed with saturated NaCl solution and dried over Na2SO4. The solvent is eliminated i.vac. and further purification is carried out by column chromatography on silica gel (EtOAc).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08618132B2 |
|---|
| 出典データセット | uspto-grants-2013_12 |
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| ORD ID | ord-1db55905c8f44b77ac647a879838b357 |
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| 出典メモ | uspto-grants-2013_12 |
|---|
