Potassium Carbonate → HCID 24206025, Verbindung

HRID 1944989Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1944989
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:12])[CH2:10]Cl)=[C:4]([C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:20])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[N:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1>CC(C)=O.C(OCC)(=O)C.CCCCCC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:12])[CH2:10][N:37]2[CH2:38][CH2:39][N:34]([C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][N:28]=3)[CH2:35][CH2:36]2)=[C:4]([C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:20])[CH:3]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 844102,4'-Dichloro-2'-o-chlorobenzoylacetanilideHCID 944591-(2-Pyridyl)piperazine

Produkt 1

HCID 24206025HCID 24206025, VerbindungAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 21226206Ethyl acetate hexaneLösungsmittel

Versuchsvorschrift

To a compound of N1-[4-chloro-2-(2-chlorobenzoyl)phenyl]-2-chloroacetamide (500 mg, 1.46 mmol) in dry acetone (20 mL) was added anhydrous potassium carbonate (1 g, 7.30 mmol) and 1-(2-pyridyl)piperazine (238 mg, 1.46 mmol). The reaction mixture was refluxed for 24 h and the reaction was monitored by TLC using ethyl acetate-hexane (6:4) as a solvent system. The potassium carbonate was then removed by suction filtration and the solvent was evaporated under vacuum to afford the crude product. This was further purified by column chromatography using ethyl acetate:hexane (6:4) as a solvent system to obtain the pure product 6a (585 mg, 86% yield).

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 24 h
  2. customThe potassium carbonate was then removed by suction filtration
  3. customthe solvent was evaporated under vacuum
  4. customto afford the crude product
  5. customThis was further purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-65c3913079284ac69f414a79de9611e8
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394954B2

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