Malononitrile → HCID 178509191、化合物

HRID 2304445ノート

反応式

HRID 2304445 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][N:8]=[C:9]([C:12]#[N:13])[C:10]#[N:11])[CH:2]=1.NC1C=NC=CC=1.C(#N)CC#N.O.[NH2:27][NH2:28]>C(O)C>[NH2:13][C:12]1[C:9](=[N:8][NH:7][C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[C:10]([NH2:11])=[N:28][N:27]=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

This compound was prepared using 2-[(pyridin-3-yl)hydrazono]malononitrile (342 mg, 2 mmole), which was derived from 3-aminopyridine (940 mg, 10 mmole)) and malononitrile (858 mg, 13 mmol) as described in Example 8, and hydrazine hydrate (110 mg, 2.2 mmole) 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 room 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. customThis compound was prepared
  2. customSolids had not formed
  3. temperatureafter heating
  4. customthe reaction at 80° C. for 40 minutes
  5. customthe solvent was evaporated
  6. customThe product was obtained after
  7. customupon re-crystallization from ethanol as a yellow solid (150 mg)

出典と根拠

ORDレコード
ord-e2ab4bcea0a949c587551910aa0cccb6
出典データセット
uspto-grants-2002_08
特許番号
US06436915B1

反応ノート

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