참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| 반응물 | HCID 178501210 | HCID 178501210 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | HCID 178501253 | HCID 178501253 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737161B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-f13ca10a3f374ab6b0ddea3ebea60e36 |
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| 출처 메모 | uspto-grants-2010_06 |
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