Water → Ethyl N-(2-buten-1-yl)-N-(2,2-dimethoxyethyl)-carbamate

HRID 36695Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 36695
[CH3:1][O:2][CH:3]([O:11][CH3:12])[CH2:4][NH:5][C:6](=[O:10])[O:7][CH2:8][CH3:9].[H-].[Na+].Br[CH2:16][CH:17]=[CH:18][CH3:19].O>C1(C)C=CC=CC=1>[CH2:16]([N:5]([CH2:4][CH:3]([O:2][CH3:1])[O:11][CH3:12])[C:6](=[O:10])[O:7][CH2:8][CH3:9])[CH:17]=[CH:18][CH3:19]

Komponenten

6

Edukt 4

HCID 962WaterHCID 24758Sodium hydrideHCID 1224142-Butene, 1-bromo-HCID 10921057Ethyl 2,2-dimethoxyethylcarbamate

Produkt 1

HCID 54206204Ethyl N-(2-buten-1-yl)-N-(2,2-dimethoxyethyl)-carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

89 g (0.5 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate are added dropwise to 17.5 g (0.58 mol) of NaH (80% strength in paraffin oil) in 500 ml of absolute toluene at 80° C. The mixture is then stirred for one hour and 80 g (0.59 mol) of 1-bromo-2-butene are subsequently added dropwise at 80° C. The mixture is stirred at 80° C. overnight and cooled, the salts are dissolved with water and the aqueous phase is separated off and extracted with toluene. The toluene solutions are dried over K2CO3 and concentrated and the residue is distilled.

Aufarbeitung

  1. stirringThe mixture is stirred at 80° C. overnight
  2. temperaturecooled
  3. customthe aqueous phase is separated off
  4. extractionextracted with toluene
  5. dry with materialThe toluene solutions are dried over K2CO3
  6. concentrationconcentrated
  7. distillationthe residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-7de3f40395fc4e26abc7714ca6ef2c32
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05416096

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