Potassium Carbonate → 3-(4-Aminophenylthio)-6-phenylpyridazine

HRID 55096

反応式

HRID 55096 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][CH:7]=1.[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([SH:21])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([S:21][C:2]2[N:3]=[N:4][C:5]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)=[CH:6][CH:7]=2)=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 145104-AminothiophenolHCID 885153-Chloro-6-phenylpyridazine

生成物 1

HCID 189716613-(4-Aminophenylthio)-6-phenylpyridazine収率 83%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3-Chloro-6-phenylpyridazine (0.026 moles, 5.0 g), 4-aminothiophenol (0.026 moles, 3.3 g) and potassium carbonate (0.026 moles, 3.6 g) were stirred in 250 ml ethanol for 3 days. The reaction was filtered, concentrated, ethyl acetate added, washed with water and dried over sodium sulfate. The solution was concentrated and the product purified by HPLC over silica gel eluted with 50% ethyl acetate/hexane to yield 3-(4-aminophenylthio)-6-phenylpyridazine 6.0 g, 83%. Mass Spec (FD) 279. Calculated for C16H13N3S: C, 68.79; H, 4.69; N, 15.04. Found: C, 68.87; H, 4.43 N, 15.31.

後処理

  1. filtrationThe reaction was filtered
  2. concentrationconcentrated
  3. additionethyl acetate added
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationThe solution was concentrated
  7. customthe product purified by HPLC over silica gel
  8. washeluted with 50% ethyl acetate/hexane

出典と根拠

ORDレコード
ord-ff0f66956c484b7280b40d560d9b6699
出典データセット
uspto-grants-1997_04
特許番号
US05624937

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