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Propanoic acid, 2-bromo-2-methyl-, ethyl ester → HCID 20329847, Verbindung

HRID 2058080
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2058080
[Na].[CH:2]1([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.Br[C:18]([CH3:25])([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(O)C>[CH:2]1([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:18]([CH3:25])([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:12][CH:11]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11745Propanoic acid, 2-bromo-2-methyl-, ethyl esterHCID 2412384-[(Cyclohexylimino)methyl]phenolHCID 5360545Sodium

Produkt 1

HCID 20329847HCID 20329847, VerbindungAusbeute 50,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

(a) To 70 ml of absolute ethanol is added 872 mg of sodium, and 7 g of 4-(N-cyclohexylformimidoyl)phenol is added to the solution. Subsequently, 7.4 g of ethyl 2-bromo-2-methylpropionate is further added. The mixture is refluxed under heating and with stirring for 15 hours. After distilling off the ethanol from the reaction mixture, water is added to the residue, and the solution is extracted three times with benzene. The extract is washed with water twice, with cooled dilute aqueous solution of sodium hydroxide three times and then with water twice. After drying the resulting solution over magnesium sulfate, the solvent is distilled off to give 5.54 g of ethyl 2-[4-(N-cyclohexylformimidoyl)phenoxy]-2-methylpropionate as an oil.

Aufarbeitung

  1. additionis added to the solution
  2. temperatureThe mixture is refluxed
  3. temperatureunder heating
  4. distillationAfter distilling off the ethanol from the reaction mixture, water
  5. additionis added to the residue
  6. extractionthe solution is extracted three times with benzene
  7. washThe extract is washed with water twice
  8. temperaturewith cooled dilute aqueous solution of sodium hydroxide three times
  9. dry with materialAfter drying the resulting solution over magnesium sulfate
  10. distillationthe solvent is distilled off

Quellen und Nachweise

ORD-Eintrag
ord-ab3ae68d7a6e40e59afeed458ea3b612
Quelldatensatz
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04214094

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