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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, monohydrate | HCID 168937 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Clofibric Acid | HCID 2797 | 82% |
反応手順
To a solution of 2-(4-chloro-phenoxy)-2-methyl-propionic acid ethyl ester (2.0 g, 8.24 mmol) in tetrahydrofuran (16 mL) at room temperature is added water (4 mL) followed by lithium hydroxide monohydrate (0.69 g, 16.4 mmol). The reaction is stirred for 16 h at room temperature. After this time, the mixture is diluted with water and washed with DCM. The aqueous phase is separated, acidified to pH ˜2 with 1M aqueous HCl solution and then extracted with DCM (x2). The combined organic extracts are washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure to give the title compound as a white solid (1.45 g, 82%). 1H NMR (400 MHz, CHLOROFORM-d): δ ppm 1.62 (6H, s), 6.89 (2H, d, J=9.0 Hz), 7.24 (2H, d, J=9.0 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08957063B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-8ebf3c5f299f465c8bf5d36d7c22816f |
| 出典メモ | uspto-grants-2015_02 |