関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,6-Difluorobenzonitrile | HCID 74695 | — |
| 反応物 | 2,3,5-Trifluorobenzyl alcohol | HCID 2777030 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Fluoro-6-(2,3,5-trifluorobenzyloxy)-benzonitrile | HCID 66924226 | 72.9% |
反応手順
To a cold (ice water) suspension of sodium hydride (407 mg; 10 mmol) in anhydrous DMF (4 is added a solution of 2,3,5-trifluorobenzyl alcohol (1.62 g; 10 mmol) in anhydrous DMF (5 mL) over 10 minutes. After allowing to room temperature over 1 hour, this solution is added to a cold (ice water) stirred solution of 2,6-difluorobenzonitrile (1.56 gm; 11 mmol) in anhydrous DMF (5 mL), and allowed to room temperature over 3 hours. TLC (25% EA/Hex) was incomplete so the reaction was continued at room temperature for an additional 2 hours. The reaction mixture is poured into ice water with vigorous stirring and the resulting solid is filtered, washed with water, and dried under vacuum at 40° C. for 4.5 hours to give 2.05 grams of 2-fluoro-6-(2,3,5-trifluorobenzyloxy)-benzonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09067897B2 |
|---|
| 出典データセット | uspto-grants-2015_06 |
|---|
| ORD ID | ord-d20ea2a180c9470d9b6942ac3c970e66 |
|---|
| 出典メモ | uspto-grants-2015_06 |
|---|