Water → HCID 13505933, Verbindung

HRID 279776Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 279776
[CH2:1]([O:3][C:4]([C:6]1(C(OCC)=O)[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])[CH3:2].[Cl-].[Na+].O>CS(C)=O>[CH2:1]([O:3][C:4]([CH:6]1[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])[CH3:2]

Komponenten

5

Edukt 3

HCID 962WaterHCID 5234Sodium Chloride2×HCID 13505928HCID 13505928, Verbindung

Produkt 1

HCID 13505933HCID 13505933, VerbindungAusbeute 90,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

A mixture of 66.2 g (0.18 mole) of diethyl[1-(2,4-dimethoxy-benzyl)-4-oxo-2,2-azetidine-dicarboxylate] prepared according to the preceding paragraph, 70 ml of dimethyl sulfoxide, 12.7 g (0.22 mole) of sodium chloride and 6.5 ml (0.36 mole) of water is stirred on an oil bath (temperature 170°-180° C. for 6 hours. The reaction mixture is poured into 500 ml of a saturated aqueous sodium chloride solution, extracted five times with 100 ml ethyl acetate each, the organic phase is dried over anhydrous magnesium sulfate, filtered and from the filtrate the ethyl acetate is distilled off. Thus 47.6 g of ethyl-[1-(2,4-dimethoxy-benzyl)-4-oxo-2-azetidine-carboxylate] are obtained. B.p.: 170°-176° C./0.15 Hgmm.

Aufarbeitung

  1. customprepared
  2. extractionextracted five times with 100 ml ethyl acetate each, the organic phase
  3. dry with materialis dried over anhydrous magnesium sulfate
  4. filtrationfiltered and from the filtrate the ethyl acetate
  5. distillationis distilled off

Quellen und Nachweise

ORD-Eintrag
ord-86aea116717242f48f5b6611ddc0bf3e
Quelldatensatz
uspto-grants-1986_05
Patentnummer
US04587049

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