化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 2-Propen-1-ol, 3-(3,4-dichlorophenyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Dibah | HCID 16682954 | — |
| 反応物 | Methyl 3-(3,4-dichlorophenyl)prop-2-enoate | HCID 54151376 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Propen-1-ol, 3-(3,4-dichlorophenyl)- | HCID 53709191 | 100% |
反応手順
Treat a solution of the product of Step 1 (15 g, 65 mmol) in dry THF (250 mL), kept cool in a large ambient temperature water bath, with Dibal-H (140 mL, 140 mmol, 2.15 eq) over 30 min. Stir the resulting solution for 30 min at 23° C., pour into Et2O (500 mL), treat with water (5 mL), 15% NaOH (5 mL) and water (15 mL). Stir for 5 min, dilute the mixture with Et2O (200 mL) and treat with 15% NaOH (15 mL). Add MgSO4 to cause a colorless precipitate. Remove the aluminum salts by filtration through a course glass frit. Wash the solids with Et2O (1 L) and concentrate the filtrate in vacuo to give 13.2 g (65 mmol, 99%) of 3-(3,4-dichlorophenyl)-2-propene-1-ol as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05789422 |
| 出典データセット | uspto-grants-1998_08 |
| ORD ID | ord-716fd709c60340bfaf11c3a86ab0967a |
| 出典メモ | uspto-grants-1998_08 |