関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Disodium disulfite | HCID 24346 | — |
| 反応物 | 2-Thiophenecarboxaldehyde, 5-chloro- | HCID 81700 | — |
| 反応物 | Methyl (3,4-diaminobenzenesulfonyl)acetate | HCID 57763314 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | HCID 178501896 | HCID 178501896 | — |
反応手順
14.4 747 mg (3.93 mmol) of sodium disulfite are added to a solution of 1.15 g (7.86 mmol) of 2-chlorothiophene-5-carbaldehyde and 1.92 g (7.86 mmol) of methyl (3,4-diaminobenzenesulfonyl)acetate in 25 ml of 1-methylpyrrolidone, and the mixture is stirred at 110° C. for 18 hours. Water is added to the reaction mixture, which is extracted with dichloromethane. The organic phase is dried over sodium sulfate and evaporated. The residue is stirred with water, and the resultant precipitate is filtered off, giving methyl [2-(5-chlorothiophen-2-yl)-1H-benzimidazole-5-sulfonyl]-acetate as a brown solid; ESI 371.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07566789B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-f5de34153b9b43da8657d33176101420 |
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| 出典メモ | uspto-grants-2009_07 |
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