関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1-Benzylimidazole | HCID 77918 | — |
| 反応物 | 2-Bromo-3-methylbenzoic acid | HCID 2735588 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (1-Benzyl-1H-imidazol-2-yl)(2-bromo-3-methylphenyl)methanone | HCID 66771155 | 102.3% |
反応手順
A solution of 2-bromo-3-methylbenzoic acid (2.0 g, 9.3 mmol) in thionyl chloride (4.75 ml, 65.1 mmol) was heated at 65° C., under nitrogen, for 3 h. The mixture was concentrated in vacuo and to the residue was added acetonitrile (25 ml). This solution was concentrated in vacuo and the process was repeated. To the final residue was added acetonitrile (25 ml), 1-benzylimidazole (1.62 g, 10.2 mmol) and triethylamine (1.44 ml, 10.2 mmol) and the reaction mixture was heated at 60° C., under nitrogen, for 18 h. The mixture was concentrated in vacuo and to the residue was added ethyl acetate (80 ml). The solution was washed with water (40 ml) and saturated aqueous sodium hydrogen carbonate solution (40 ml), dried (MgSO4) and concentrated in vacuo to give the title compound (3.38 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07592362B2 |
|---|
| 出典データセット | uspto-grants-2009_09 |
|---|
| ORD ID | ord-b3e311d636bc4019bca38db43e9304ee |
|---|
| 出典メモ | uspto-grants-2009_09 |
|---|