Water → 2-(2-(Dibenzylamino)ethoxy)ethanol

HRID 23855

Reaktionsgleichung

Reaktionsgleichung von HRID 23855
[NH2:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][OH:7].C(=O)([O-])[O-].[K+].[K+].O.[CH2:15](Br)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CCO>[CH2:15]([N:1]([CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[CH2:2][CH2:3][O:4][CH2:5][CH2:6][OH:7])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 13578Diglycolamine

Produkt 1

HCID 158924642-(2-(Dibenzylamino)ethoxy)ethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of 50 g (475.56 mmol) of 2-(2-amino-ethoxy)ethanol and 144.6 g (1.046 mol) of potassium carbonate in 600 ml of EtOH/60 ml of water is heated to 60° C. To this mixture is added dropwise within one hour 178.95 g (1.046 mol) of benzyl bromide and then the mixture is refluxed for 2 hours, evaporated under vacuum, the residue taken up with 1 liter of methylene chloride, and filtered off from the salts. The filtrate is concentrated under vacuum and purified by flash chromatography (silica gel/mobile phase: methylene chloride/hexane/acetone: 10/5/1).

Aufarbeitung

  1. temperaturethe mixture is refluxed for 2 hours
  2. customevaporated under vacuum
  3. filtrationfiltered off from the salts
  4. concentrationThe filtrate is concentrated under vacuum
  5. custompurified by flash chromatography (silica gel/mobile phase: methylene chloride/hexane/acetone: 10/5/1)

Quellen und Nachweise

ORD-Eintrag
ord-43a05c91ffe04d93bf0781fb633d978b
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06855309B2

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