関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(4-Methyl-2-thienyl)ethan-1-one | HCID 83654 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 生成物 | 4-Methylthiophene-2-carboxylic acid | HCID 2794584 | — |
反応手順
To an aqueous solution of sodium hypochlorite (available chlorine 5%) (92.6 mL, 143.0 mmol) at about 0° C. was added sodium hydroxide (1.14 g, 28.6 mmol) and the mixture was stirred at about 0° C. until all of the sodium hydroxide had dissolved. To this solution was added 2-acetyl-4-methylthiophene (2.0 g, 14.3 mmol) at about 0° C. After the addition was complete, the mixture was heated to about 70° C. for about 3 hours, then the solution was cooled and was carefully quenched by addition of a solution of sodium bisulfite (23 g) in water (150 mL). After stirring for about 20 minutes, the solution was acidified by addition of concentrated hydrochloric acid and the precipitate was collected by filtration and dried under high vacuum to provide the desired product. MS (DCI-NH3): m/z 160 (M+NH4)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07468371B2 |
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| 出典データセット | uspto-grants-2008_12 |
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| ORD ID | ord-3f94701b2fcd4e8ba9d9f32f00cecf91 |
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| 出典メモ | uspto-grants-2008_12 |
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