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

HRID 55096

반응식

HRID 55096 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 189716613-(4-Aminophenylthio)-6-phenylpyridazine수율 83%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ff0f66956c484b7280b40d560d9b6699
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624937

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