Water → HCID 54109521, Verbindung

HRID 258700Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 258700
[H-].[Na+].[S:3]([C:7]1[NH:8][CH:9]=[CH:10][N:11]=1)([CH3:6])(=[O:5])=[O:4].Cl[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15].O>CN(C)C=O.C(Cl)Cl>[S:3]([C:7]1[N:8]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:9]=[CH:10][N:11]=1)([CH3:6])(=[O:5])=[O:4]

Komponenten

7

Edukt 4

HCID 962WaterHCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 993902-(Methylsulfonyl)imidazole

Produkt 1

HCID 54109521HCID 54109521, VerbindungAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

Sodium hydride (50% suspension in mineral oil) (5.04 g.) is added, under a nitrogen atmosphere, to a solution of 2-mesyl-imidazole (15.3 g.) in dimethylformamide (130 cc.). Ethyl chloroacetate (12.9 g.) is then added. Reaction is allowed to take place for 20 hours, with stirring, at a temperature of about 20° C. The reaction mixture is then poured into water (4 liters) and extraction is effected using methylene chloride (1 liter). The methylene chloride extracts are washed with water, dried over sodium sulphate, treated with decolorising charcoal and then concentrated to dryness under reduced pressure (0.5 mm.Hg) to yield ethyl (2-mesyl-imidazol-1-yl)-acetate (21.4 g.) in the form of an oil.

Aufarbeitung

  1. customReaction
  2. customfor 20 hours
  3. washThe methylene chloride extracts are washed with water
  4. dry with materialdried over sodium sulphate
  5. additiontreated with decolorising charcoal
  6. concentrationconcentrated to dryness under reduced pressure (0.5 mm.Hg)

Quellen und Nachweise

ORD-Eintrag
ord-8d03edfc897a427fbd339f239b7ac215
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04034088

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