Malononitrile → HCID 178509191、化合物

HRID 2095147ノート

反応式

HRID 2095147 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 178509191HCID 178509191、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-372d82534608498caf36ec3cc81c0c25
出典データセット
uspto-grants-2013_05
特許番号
US08445694B2

反応ノート

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