関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| 反応物 | HCID 178501210 | HCID 178501210 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 178501253 | HCID 178501253 | — |
反応手順
Methyl trans-4-aminocyclohexanecarboxylate hydrochloride (4.08 g) obtained in Reference Example 2(1) is suspended in chloroform (50 ml), and thereto is added triethylamine (8.8 ml) under ice-cooling. Subsequently, a solution of 3-chloropropanesulfonyl chloride (3.35 ml) in chloroform (20 ml) is added dropwise over 20 minutes under the same temperature. After stirring for 2 hours at room temperature, 5% hydrochloric acid is added to the reaction solution and the mixture is extracted with chloroform. The organic layer is washed with saturated brine, dried over sodium sulfate and evaporated to remove the solvent under reduced pressure. The resulting residue is suspended in diisopropylamine, and filtered to collect precipitates to give methyl trans-4-{[(3-chloropropyl)sulfonyl]amino}cyclohexanecarboxylate (6.14 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737161B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-f13ca10a3f374ab6b0ddea3ebea60e36 |
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| 出典メモ | uspto-grants-2010_06 |
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