関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1-Tetradecanol | HCID 8209 | — |
| 反応物 | 4-Nitrobenzoyl chloride | HCID 8502 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tetradecyl 4-nitrobenzoate | HCID 591245 | — |
反応手順
Under a nitrogen atmosphere, a mixture of 1-tetradecanol (96.3 grams, 449 millimoles (mmol), pyridine (40 milliliters), and dichloromethane (1000 milliliters) was heated to 30° C. 4-Nitrobenzoyl chloride (100 grams, 539 mmol) was added in portions over a twenty minute period. The reaction mixture was heated to reflux for sixteen hours. The reaction mixture was then washed twice with water (2×500 milliliters). The organic layer was concentrated under reduced pressure to a yellow solid. One thousand (1000) milliliters of hexane was added, and the mixture was heated to reflux. The mixture was cooled and concentrated to yield a yellow solid that was filtered. The yellow solid was recrystallized twice from ethanol to obtain 77.0 grams of tetradecyl 4-nitrobenzoate as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07765698B2 |
|---|
| 出典データセット | uspto-grants-2010_08 |
|---|
| ORD ID | ord-db9fe98de9e94fafb985403d8ff18508 |
|---|
| 出典メモ | uspto-grants-2010_08 |
|---|