関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Acetaminophen | HCID 1983 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-(4-Aminophenoxy)-2-methylpropanoic acid | HCID 2774958 | — |
| 生成物 | 2-(4-Acetamidophenoxy)-2-methylpropanoic acid | HCID 14879855 | 60% |
反応手順
FIG. 2A illustrates a reaction scheme for preparing 2-(4-aminophenoxy)-2-methyl propionic acid, a compound that is useful as a precursor in the preparation of Group I compounds. In accordance with the scheme of FIG. 2A, 8 grams (g) (0.2 mol) of pulverized sodium hydroxide is added to a suspension of 5.28 g (0.035 mol) of p-acetamidophenol in 23 ml (0.4 mol) of acetone. The reaction mixture is stirred at room temperature for 1/2 hour. Subsequently, 3.58 g (0.03 mol) of chloroform is added dropwise over the course of 30 minutes. The reaction mixture is stirred overnight at room temperature and acetone is removed under vacuum. The residue is dissolved in water (10 ml), followed by acidification with 37% hydrochloric acid (HCl) to produce a pale yellow precipitate of 2-(4-acetaminophenoxy)-2-methyl propionic acid (5 g, 60% yield), crystallized from methanol, mp 69°-71° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05731454 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-8d4bf2d31e824543ac5f1049cd6477c4 |
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| 出典メモ | uspto-grants-1998_03 |
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