関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,2-Dibromobenzene | HCID 11414 | — |
| 反応物 | But-3-enyl-((S)-1-phenyl-ethyl)-amine | HCID 10559173 | — |
| 触媒 | HCID 178419072 | HCID 178419072 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 3-Bromodiphenyl ether | HCID 96165 | 53% |
反応手順
1-Bromo-3-phenoxy-benzene (A) A mixture of dibromobenzene (3 g, 12.75 mmol), phenol (1 g, 10.6 mmol), copper(I) oxide (152 mgs, 1 mmol), and cesium carbonate (3.46 g, 10.6 mmol) in 8 mL of NMP is heated at 195° C. for 20 minutes in a microwave. The heterogeneous mixture is filtered through a bed of Celite and the residue is washed with EtOAc (1×20 mL). The filtrate is diluted with 1N NaOH (200 mL) and extracted with EtOAc (3×100 mL). The organics were combined, dried over Na2SO4, filtered and concentrated under reduced pressures to give crude product as a yellow oil which is purified by column chromatography (100% hexanes) to give 1-bromo-3-phenoxy-benzene as a colorless oil (1.4 g, 53%). LCMS m/z 250 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07419975B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-1ec6e12902da4d58a1a61dc46f845bd1 |
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| 出典メモ | uspto-grants-2008_09 |
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