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Lithium hydroxide, monohydrate → 4-Fluoro-3-methoxybenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | Methyl 4-fluoro-3-methoxybenzoate | HCID 592847 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Fluoro-3-methoxybenzoic acid | HCID 598436 | — |
反応手順
4-Fluoro-3-methoxybenzoic acid methyl ester (2.55 g, 13.85 mmol) (from Example 34a supra) was dissolved in a mixture of tetrahydrofuran (140 mL) and water (70 mL). Lithium hydroxide monohydrate (5.8 g, 138.5 mmol) was added and the mixture was heated at reflux for 3.5 hours. After quenching with 1 N aqueous hydrochloric acid (150 mL), the solution was extracted with dichloromethane. The phases were separated and the organic layer was dried over anhydrous sodium sulfate. Concentration under reduced pressure gave 4-fluoro-3-methoxybenzoic acid as an off-white solid. (Yield 2.26 g, 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07115740B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-8965fad0d61e4d788294bca84dced858 |
| 出典メモ | uspto-grants-2006_10 |