関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methyl 3-amino-2-thiophenecarboxylate | HCID 89652 | — |
| 反応物 | 4-t-Butylbenzenesulfonyl chloride | HCID 139882 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | Methyl 3-(4-tert-butylphenylsulfonamido)thiophene-2-carboxylate | HCID 8015643 | 92.5% |
反応手順
In an appropriate vessel, methyl 3-aminothiophene-2-carboxylate (2.5 g; 15.9 mmol) was combined with 4-tert-butylbenzene sulfonyl chloride (3.70 g; 15.9 mmol) and dissolved by addition of pyridine (5.00 mL; 63.2 mmol). The reaction mixture was heated at 65° C. for 2 hours cooled to room temperature, diluted with aqueous hydrochloric acid (100 mL; 2M) and extracted with dichloromethane (3×30 mL). The combined organic extracts were washed with aqueous hydrochloric acid (100 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting crude solid was recrystallized from a minimal amount of isopropanol to give the title product as a yellow solid (5.2 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08178699B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-99d88049fc4f408e9f63ac647e8fb6b1 |
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| 出典メモ | uspto-grants-2012_05 |
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