化工社化工社 化学情報印刷レポート · 研究参考用
Clofibrate → Clofibric Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Clofibrate | HCID 2796 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Clofibric Acid | HCID 2797 | 20.7% |
反応手順
To a solution of 2-(4-Chloro-phenoxy)-2-methyl-propionic acid ethyl ester (6 g, 24.79 mmol) in THF (20 ml) was added a solution of LiOH (3 g, 74.38 mmol) in H20 (4 ml). The resulting solution was stirred at room temperature for 12 hours. After evaporation of the solvent, the residue was diluted with ethyl acetate (100 ml); cool to 0° C., acidified with 1N HCl (PH˜3-4). The organic phase were washed with, brine (20 ml) and dried over Na2SO4. After evaporation, the residue was purified by flash chromatography (1:1 hexanes/EtOAc) to give 2-(4-Chloro-phenoxy)-2-methyl-propionic acid (1.1 g, 20%). 1H NMR (400 MHz, CDCl3): δ 1.60 (s, 6H), 6.85 (d, J=8.7 Hz, 2H), 7.22 (d, J=8.7 Hz, 2H). MS (EI) m/z: 215.5 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08940900B2 |
| 出典データセット | uspto-grants-2015_01 |
| ORD ID | ord-850b74c115a340d2bf0a5b20f5497a0d |
| 出典メモ | uspto-grants-2015_01 |