참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Cyclohexanecarboxylic acid | HCID 7413 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 5-Fluoro-2-hydrazinylpyridine | HCID 19916786 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Cyclohexanecarboxylic acid N'-(5-fluoro-pyridin-2-yl)-hydrazide | HCID 86686727 | 62% |
반응 단계
To a solution of 5-fluoro-2-hydrazinyl-pyridine (for reference procedure see WO 2010 022076, which is incorporated herein by reference in its entirety; 1.00 g, 7.87 mmol), cyclohexane carboxylic acid (1.21 g, 9.44 mmol), and HOBt.H2O (166 mg, 0.787 mmol) at 0° C. under N2 was added EDC (1.81 g, 9.44 mmol), then the mixture stirred at 0° C. for 15 min, and at RT for 17 h. Water was added, then the organics isolated, cooled to 0° C., then the resulting suspension filtered to leave the title compound as a white solid (1.16 g, 62%). 1H NMR (400 MHz, CDCl3): 1.21-1.38 (3H, m), 1.45-1.55 (2H, m), 1.66-1.73 (1H, m), 1.80-1.96 (4H, m), 2.22 (1H, tt, J 11.6, 3.5 Hz), 6.62-6.66 (2H, m), 7.29 (1H, ddd, J 9.2, 7.9, 3.1 Hz), 7.55 (1H, d, J=4.2 Hz), 8.03 (1H, d, J=2.9 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08835431B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-0438aecd2bd8479eb2f5017913471c2e |
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| 출처 메모 | uspto-grants-2014_09 |
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