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Methanol → 3-Hydroxy-5-(trifluoromethyl)thiophene-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl 3-hydroxy-5-(trifluoromethyl)thiophene-2-carboxylate | HCID 2759855 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Hydroxy-5-(trifluoromethyl)thiophene-2-carboxylic acid | HCID 2759348 | 65% |
反応手順
A mixture of 5B (2.38 g) and methanol (20 ml) was added to a stirred solution of sodium hydroxide (1.68 g) in water (20 ml). The reaction mixture was heated at reflux for 3 hours. The reaction mixture was cooled to room temperature and concentrated in vacuo. The concentrate was cooled to 5° C. and acidified with concentrated HCI (3.5 ml). The resulting suspension was stirred at 5° C. for 30 minutes. The solid was collected by filtration, washed with water, then dried in vacuo at 35-40° C. to give the free acid (1.45 g, 65 %).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06130188 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-6dbbda8ea60b48b6b4d1fafd783ae10e |
| 出典メモ | uspto-grants-2000_10 |