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Water → 4-(2,3,4-TRIMETHOXYPHENYL)-4-OXOBUTYRIC ACID
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Oxo-4-(2,3,4-trimethoxy-phenyl)-butyric acid methyl ester | HCID 44720458 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(2,3,4-TRIMETHOXYPHENYL)-4-OXOBUTYRIC ACID | HCID 10945432 | 94% |
反応手順
5.95 g of sodium hydroxide was dissolved in 200 mL of methanol in a 500 mL round bottom flask. The reaction mixture was cooled to room temperature and 55 (6.78 g, 22.90 mmol) was added followed by 20 mL of water and 100 mL of methanol and the reaction mixture was refluxed for 30 min. The solvent was evaporated under reduced pressure and the reaction mixture was neutralized with dilute hydrochloric acid and the reaction mixture was extracted with ether (100×3) and the combined organic phases were washed with water and dried over sodium sulfate and solvent evaporated under reduced pressure. The crude product was purified by column chromatography (20:80 EtOAc:Hexanes) to yield 5.43 g of 56 as tan colored solid (94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429681B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-8585746e039b4684ae00cb3e388f6193 |
| 出典メモ | uspto-grants-2008_09 |