Malononitrile → HCID 178509191, 화합물

HRID 2095147노트

반응식

HRID 2095147 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]=1

참가 물질

6

반응물 4

HCID 8010MalononitrileHCID 100093-AminopyridineHCID 24654Hydrazine hydrate (1:1)HCID 21955014Pyridin-3-ylcarbonohydrazonoyl dicyanide

생성물 1

HCID 178509191HCID 178509191, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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

  1. customSolids had not formed
  2. temperatureafter heating
  3. customthe reaction at 80° C. for 40 minutes
  4. customthe solvent was evaporated
  5. customThe product was obtained after
  6. customupon re-crystallization from ethanol as a yellow solid (150 mg)

출처 및 근거

ORD 기록
ord-372d82534608498caf36ec3cc81c0c25
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445694B2

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