化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl 4-(1H-pyrazol-1-YL)benzoate → (4-(1H-Pyrazol-1-yl)phenyl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 4-(1H-pyrazol-1-YL)benzoate | HCID 973146 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Calcium Chloride | HCID 5284359 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (4-(1H-Pyrazol-1-yl)phenyl)methanol | HCID 2776480 | 83.5% |
反応手順
To a solution of ethyl 4-(1H-pyrazol-1-yl)benzoate (73.7 g) in THF (500 mL) were added sodium borohydride (19.5 g) and calcium chloride (56.8 g) under ice-cooling, and the mixture was stirred at room temperature for 16 hr, and then heated with reflux for 2 days. The reaction mixture was diluted with 1N hydrochloric acid, and the mixture was extracted with ethyl acetate (×4). The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was washed with tert-butyl methyl ether to give the title compound (49.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09315458B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-5166db553cfa4411a7c1264e42643cf0 |
| 出典メモ | uspto-grants-2016_04 |