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Citric Acid → 1-Methyl-1H-benzimidazole-5-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 1-methyl-1h-benzimidazole-5-carboxylate | HCID 965320 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 1-Methyl-1H-benzimidazole-5-carboxylic acid | HCID 4913063 | 86.2% |
反応手順
Ethyl 1-methyl-1H-benzimidazole-5-carboxylate (800 mg, 3.92 mmol) prepared in the Step 1-1-4 was suspended in 2-propanol (10 ml), and a 1 mol/L sodium hydroxide aqueous solution (10 ml) was added thereto. The mixture was heated under reflux for one hour. After being allowed to cool, the mixture was neutralized with 1 mol/L hydrochloric acid. The resulting mixture was then acidified with citric acid, separated by filtration, and washed with a small quantity of water. Then, the resulting product was subjected to through circulation drying overnight to give the title compound (595 mg, 86%) as a gray powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09200008B2 |
| 出典データセット | uspto-grants-2015_12 |
| ORD ID | ord-919dfc4e6f544d878b2785e4332178c9 |
| 出典メモ | uspto-grants-2015_12 |