Potassium Carbonate → 2-(4-Aminophenylthio)quinoline

HRID 55060

反応式

HRID 55060 の反応式
Cl[C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([SH:19])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([S:19][C:2]2[CH:11]=[CH:10][C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 119282-ChloroquinolineHCID 145104-Aminothiophenol

生成物 1

HCID 226371302-(4-Aminophenylthio)quinoline収率 40%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Chloroquinoline (0.04 moles, 6.54 g), 4-aminothiophenol (0.04 moles, 5.0 g) and potassium carbonate (0.04 moles, 5.52 g) were stirred at room temperature in 200 ml of ethanol for 18 hr. The reaction mixture was concentrated, ethyl acetate was added and the solution washed with water, dried over sodium sulfate and concentrated. The product was purified by HPLC over silica gel eluted with ethyl acetate/hexane to yield 2-(4-aminophenylthio)quinoline 4.0 g, 40%. Mass Spec (FD) 252. Calculated for C15H12N2S: C, 71.40; H, 4.79, N, 11.10. Found: C, 71.11; H, 4.98 N, 11.20.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionethyl acetate was added
  3. washthe solution washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe product was purified by HPLC over silica gel
  7. washeluted with ethyl acetate/hexane

出典と根拠

ORDレコード
ord-3e7a9532a7bd4fcb9a6212a91312e2e6
出典データセット
uspto-grants-1997_04
特許番号
US05624937

関連ノート

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