関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Benzoic acid, 2-fluoro-, ethyl ester | HCID 67953 | — |
| 反応物 | ((1H-imidazol-2-yl)methyl)dimethylamine | HCID 11457689 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2-Dimethylaminomethyl-imidazol-1-yl)-benzoic acid ethyl ester | HCID 89650133 | 18% |
反応手順
A mixture of 2-fluoro-benzoic acid ethyl ester (200 mg; 1.19 mmol; 10 eq.), (1H-imidazol-2-ylmethyl)-dimethyl-amine (149 mg; 1.19 mmol; 1 eq.) and cesium carbonate (775 mg; 2.38 mmol; 2 eq.) in DMSO (3 mL) was stirred at 120° C. for 16 hours. The mixture was diluted with EA, washed with water (3×), dried over magnesium sulfate and concentrated in vacuo to afford the title compound (58 mg, 18%) as a white solid. HPLC (max plot) 95.7%; Rt 1.80 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09403835B2 |
|---|
| 出典データセット | uspto-grants-2016_08 |
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| ORD ID | ord-d63f11815a5f4e159cf2a7763df8b5aa |
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| 出典メモ | uspto-grants-2016_08 |
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