関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | 3-Pyridineacetic acid, hydrochloride (1:1) | HCID 2723724 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Pyridineethanol | HCID 80515 | 34.5% |
反応手順
A round-bottomed flask equipped with a magnetic stirring bar is charged with 13.9 g (0.08 mol) of (3-pyridinyl)acetic acid, hydrochloride salt (Aldrich Chemical Co.) and 400 ml of tetrahydrofuran (THF) under a nitrogen atmoshphere. To this solution lithium aluminum hydride (6.0 g, 0.16 mol) is added at room temperature for 24 hr. Saturated aqueous sodium sulfate is then added dropwise until the mixture becomes white. The solution is dried over anhydrous sodium sulfate. After filtration and concentration the resulting yellow oil is purified by 324 g of HPLC grade silica gel, eluting with ethyl acetate-hexane-ethanol (10:1:1) and collecting 40 ml fractions. Fractions 21-43 homogeneous on TLC are combined and concentrated in vacuo to give a light yellow oil (3.4 g, 34%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04789745 |
|---|
| 出典データセット | uspto-grants-1988_12 |
|---|
| ORD ID | ord-dd4d3671609c47b3b9e1a27e66c336f8 |
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| 出典メモ | uspto-grants-1988_12 |
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