関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Bromo-4-fluorobenzonitrile | HCID 123579 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 68854444 | HCID 68854444 | — |
反応手順
3-Bromo-4-fluorobenzonitrile (10.0 g, 50 mmol, 1 eq) and imidazole (5.1 g, 75 mmol, 1.5 eq) are dissolved in dimethylformamide (100 ml) and carefully admixed with sodium hydride (60% in mineral oil, 3.0 g, 75 mmol, 1.5 eq) under nitrogen at room temperature. The mixture is stirred at 100° C. for 4 hours. After cooling to room temperature, water (10 ml) is added and the mixture is evaporated to dryness. The residue is washed with water and petroleum ether and purified by column chromatography (silica gel, methyl tert-butyl ether/ethyl acetate gradient).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08877937B2 |
|---|
| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-ebad00ea2dd64a198e30f0f28e1bf016 |
|---|
| 出典メモ | uspto-grants-2014_11 |
|---|