참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 6-Chloronicotinic acid | HCID 79222 | — |
| 반응물 | (1-Aminocyclohexyl)methanol | HCID 409153 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | HCID 178526939 | HCID 178526939 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6-chloro-N-[1-(hydroxymethyl)cyclohexyl]nicotinamide | HCID 11950360 | 113.6% |
반응 단계
Triethylamine (2.2 ml, 16.12 mmol, 2 eq), hydroxybenzotriazole hydrate (0.217 g, 1.61 mmol, 0.2 eq), and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.7 g, 8.87 mmol, 1.1 eq) are added to a cold (ice bath) solution of 6-chloronicotinic acid (1.27 g, 8.06 mmol, 1 eq) and (1-aminocyclohexyl)methanol (1.04 g, 8.06 mmol, 1 eq) in dichloromethane (80 ml), stirred 30 min at 0° C. and then at room temperature for 1 h. The organic layer is then washed with water, with a saturated solution of aqueous sodium hydrogenocarbonate and dried over magnesium sulfate. The solvent is finally removed to give 2.46 g of a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07863450B2 |
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| 출처 데이터셋 | uspto-grants-2011_01 |
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| ORD ID | ord-624893e5f2aa4271acb0cfd5c42242e3 |
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| 출처 메모 | uspto-grants-2011_01 |
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