Malononitrile → HCID 178509191, 화합물
반응식
N1C=CC=C(N[N:8]=[C:9]([C:12]#[N:13])[C:10]#[N:11])C=1.[NH2:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1.C(#N)CC#N.O.[NH2:27][NH2:28]>C(O)C>[N:17]1[CH:18]=[CH:19][CH:20]=[C:15]([NH:14][N:8]=[C:9]2[C:10]([NH2:11])=[N:28][N:27]=[C:12]2[NH2:13])[CH:16]=1참가 물질
실험 절차
4-(pyridin-3-ylhydrazono)-4H-pyrazole-3,5-diamine was prepared using 2-[(pyridin-3-yl)hydrazono]malononitrile (342 mg, 2 mmol), which was derived from 3-aminopyridine (940 mg, 10 mmol)) and malononitrile (858 mg, 13 mmol), and hydrazine hydrate (110 mg, 2.2 mmol) in ethanol. Solids had not formed after heating the reaction at 80° C. for 40 minutes, however, analysis of the reaction solution by TLC indicated that no starting material remained. The solution was allowed to cool to ambient temperature and the solvent was evaporated. The product was obtained after upon re-crystallization from ethanol as a yellow solid (150 mg); 1H NMR (ppm, DMSO-d6): 6.18 (br., s, 4H), 7.20 (dd, 1H), 8.00 (dd, 1H), 8.38 (d, 1H), 8.85 (s, 1H), 10.77 (br., s, 1H).
후처리
- customSolids had not formed
- temperatureafter heating
- customthe reaction at 80° C. for 40 minutes
- customthe solvent was evaporated
- customThe product was obtained after
- customupon re-crystallization from ethanol as a yellow solid (150 mg)
출처 및 근거
- ORD 기록
- ord-934fea9c522348c69c8b0739d68f1937
- 출처 데이터셋
- uspto-grants-2011_01
- 특허 번호
- US07875728B2
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