참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Cyclohexanol, 1-(aminomethyl)-, hydrochloride (1:1) | HCID 3084332 | — |
| 반응물 | 2,4-Dichloro-5,6-dimethyl-3-nitropyridine | HCID 12109123 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-{[(2-Chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]methyl}cyclohexanol | HCID 57515431 | — |
반응 단계
A 500 mL round bottom flask was charged with 2,4-dichloro-5,6-dimethyl-3-nitropyridine (6.00 g, 27.1 mmol), 1-aminomethyl-1-cyclohexanol hydrochloride (4.94 g, 29.8 mmol), and N,N-dimethylformamide (200 mL). The solution was cooled to 0° C. and triethylamine (8.31 mL, 59.6 mmol) was added dropwise. The solution was heated to 35° C. for 3 d. The volatiles were removed under reduced pressure and the resulting oil was partitioned between dichloromethane (300 mL) and water (50 mL). The organic layer was washed with water (50 mL) and brine (30 mL), dried over MgSO4, filtered, concentrated under reduced pressure, and dried under vacuum to yield 1-{[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]methyl}cyclohexanol that was used without further manipulation in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541438B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-81ac5fe2e5f84b67a570f755714c6630 |
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| 출처 메모 | uspto-grants-2013_09 |
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