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Sulfuric Acid → Methyl 3-hydroxy-5-(trifluoromethyl)thiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Methyl Thioglycolate | HCID 16907 | — |
| 反応物 | 3-Methoxy-4,4,4-trifluoro-2-butenoic acid ethyl ester | HCID 2758867 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 3-hydroxy-5-(trifluoromethyl)thiophene-2-carboxylate | HCID 2759855 | 65% |
反応手順
A solution of 1 M potassium hydroxide in methanol (30 ml) is added to a cooled mixture of 5A (4.6 g), methyl thioglycolate (2.46 g) and methanol (10 ml). The resulting reaction mixture was stirred for 24 hours at room temperature. Then the mixture was poured on ice and acidified with 6N sulfuric acid (pH=2). The mixture is extracted with diethyl ether twice. The combined organic phases were washed with water and dried. The mixture was concentrated and the residue is distilled under reduced pressure to yield the product as a clear liquid (3.4 g, 65 %) with a boiling point of 42-45 ° C. at 0.10 mm.
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-42755b791c124733afbbde245024a551 |
| 出典メモ | uspto-grants-2000_10 |