Potassium Carbonate → HCID 24206026, Verbindung

HRID 1944990Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1944990
[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]=[N: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[N:28]=[CH:33][CH:32]=[CH:31][N:30]=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 887471-(2-Pyrimidinyl)piperazine

Produkt 1

HCID 24206026HCID 24206026, VerbindungAusbeute 83,7 %

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-pyrimidinyl)piperazine (239 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 6b (575 mg, 83% 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-105a4f962699478ebf480ca6f5ed2088
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394954B2

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