化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Methyl 4-fluoro-2-(methoxymethoxy)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Fluorosalicylic acid | HCID 67661 | — |
| 生成物 | Methyl 4-fluoro-2-(methoxymethoxy)benzoate | HCID 58437341 | — |
反応手順
To a solution of 4-fluoro-2-hydroxybenzoic acid (3.0 g) in N,N-dimethylformamide (5 mL) were added sodium hydride (60% 1.0 g) and (chloromethyl)methyl ether (2.1 g) at room temperature, and this mixture was stirred for 48 hours at the same temperature. This reaction mixture was poured into 2 mol/L hydrochloric acid and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (0.22 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829040B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-634103d164394d749f715694d9554186 |
| 出典メモ | uspto-grants-2014_09 |