Ethylene Glycol → Tertiary butoxymethyl diethylene glycol

HRID 127665

Reaktionsgleichung

Reaktionsgleichung von HRID 127665
[CH2:1]([OH:4])[CH2:2][OH:3].[CH3:5][C:6]([O:9][CH2:10][CH:11]1[O:13][CH2:12]1)([CH3:8])[CH3:7].[OH-].[Na+]>B(F)(F)F.CCOCC.ClCCl>[C:6]([O:9][CH2:10][CH:11]([OH:13])[CH2:12][O:3][CH2:2][CH2:1][OH:4])([CH3:5])([CH3:7])[CH3:8]

Komponenten

6

Edukt 3

HCID 174Ethylene GlycolHCID 14798Sodium HydroxideHCID 243142-((1,1-Dimethylethoxy)methyl)oxirane

Produkt 1

HCID 20285608Tertiary butoxymethyl diethylene glycolAusbeute 71 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8000Boron trifluoride etherateKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of ethylene glycol (248 g, 4 moles) and boron trifluoride etherate catalyst (1 ml) in dichloromethane (20 ml) preheated to 45° C. was added t-BGE (130 g, 1 mole) dropwise at such a rate so as to maintain a gentle reflux. After completion of addition, stirring was continued for about 15 hours. The solution was then adjusted to pH 7.5 by addition of sodium hydroxide and the product removed by distillation. Tertiary butoxymethyl diethylene glycol was obtained in 71 percent yield having a boiling point of 105° C.-115° C./1 mm.

Aufarbeitung

  1. custompreheated to 45° C.
  2. temperatureto maintain a gentle reflux
  3. additionAfter completion of addition
  4. customthe product removed by distillation

Quellen und Nachweise

ORD-Eintrag
ord-203857138ae24d558113da98a74e02ca
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04256859

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