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Water → HCID 19972395, Verbindung

HRID 2259911
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2259911
[Cl:1][CH2:2][CH2:3][CH2:4][S:5]([C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1)(=[O:7])=[O:6].[CH3:26][O:27][C: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.O>CN(C)C=O>[ClH:1].[CH3:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[N:34]1[CH2:39][CH2:38][N:37]([CH2:2][CH2:3][CH2:4][S:5]([C:8]2[C:17]3[O:16][C:15]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=3[CH:11]=[CH:10][CH:9]=2)(=[O:7])=[O:6])[CH2:36][CH2:35]1
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Komponenten

5

Edukt 3

HCID 962WaterHCID 13461-(2-Methoxyphenyl)piperazineHCID 19972358HCID 19972358, Verbindung

Produkt 1

HCID 19972395HCID 19972395, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 3.8 g of Intermediate XXXV and 4 g of 1-(2-methoxyphenyl)-piperazine in 40 ml of dimethylformamide was heated at 60° C. for 7 hours. After cooling to 20°-25° C., the reaction mixture was poured into 500 ml of water and extracted with dichloromethane. The organic extracts were washed with water and dried on anhydrous sodium sulfate, and the solvent was then evaporated off in vacuo. The residue was purified by flash chromatography on silica gel, eluting with ethyl acetate:petroleum ether (1:1). The base of the title compound was obtained. It was dissolved in ethanol and one equivalent of ethanolic hydrogen chloride was added to give 4.5 g of the title compound, m.p. (215) 226°-228C.

Aufarbeitung

  1. temperatureAfter cooling to 20°-25° C.
  2. extractionextracted with dichloromethane
  3. washThe organic extracts were washed with water
  4. dry with materialdried on anhydrous sodium sulfate
  5. customthe solvent was then evaporated off in vacuo
  6. customThe residue was purified by flash chromatography on silica gel
  7. washeluting with ethyl acetate:petroleum ether (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-87bb0e3c53624a0bab68cbadc2456d3b
Quelldatensatz
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05474994

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