Water → HCID 69497924, Verbindung

HRID 460666

Reaktionsgleichung

Reaktionsgleichung von HRID 460666
[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[CH:5]=[C:6]1[CH2:10][CH2:9][NH:8][C:7]1=[O:11].[H-].[Na+].[CH3:18][O:19][CH2:20][CH2:21]Cl.O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[CH:5]=[C:6]1[CH2:10][CH2:9][N:8]([CH2:21][CH2:20][O:19][CH3:18])[C:7]1=[O:11]

Komponenten

6

Edukt 4

HCID 962WaterHCID 123162-Chloroethyl methyl etherHCID 24758Sodium hydrideHCID 2641593-(2'-Methoxybenzylidene)-2-pyrrolidone

Produkt 1

HCID 69497924HCID 69497924, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The intermediate 3-(2′-methoxybenzylidene)-2-pyrrolidone (5.0 g) obtained in Example 317 was dissolved in dimethylformamide (50 ml) and sodium hydride (0.99 g) was added under ice-cooling. The mixture was stirred at room temperature for 30 min. To the reaction mixture was again added 2-methoxyethyl chloride (2.3 ml) under ice-cooling, and the mixture was stirred at room temperature for 1 hr and at 70° C. for 1 hr. After cooling, the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give an oily title compound (2.8 g).

Aufarbeitung

  1. temperaturecooling
  2. temperaturecooling
  3. stirringthe mixture was stirred at room temperature for 1 hr and at 70° C. for 1 hr
  4. temperatureAfter cooling
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2f4d75ed6b214df99216f686092b13cf
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07196199B2

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