Reaktion #518082

ord-31af3664bd43479087ff6b8e76be7b0d

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the completion of dropwise addition
  2. 2
    workup.STIRRINGthe mixture was stirred for about 2 hours
  3. 3
    Filtrationa precipitated salt was filtered off
  4. 4
    Sonstigecondensed
  5. 5
    workup.DISTILLATIONpurified by a vacuum distillation

Vorschrift

20.4 g (0.51 mol) of NaOH pellets were added to 100 g (0.34 mol) of 1,3-bis[2-(2-methoxyethoxy)ethoxy]-2-propanol resulting from Step 1. 48.2 g (0.51 mol) of 2-chloroethylmethylether was dropwise added in small portions while stirring at 60° C. After the completion of dropwise addition, the mixture was stirred for about 2 hours and a precipitated salt was filtered off, the filtrate was condensed and purified by a vacuum distillation to give 102 g of 1,3-bis[2-(2-methoxyethoxy)ethoxy]-2-(2-methoxyethoxy)propane (E) (yield: 85%). The distillation temperature was from 155 to 161° C./0.2 mmHg.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06656252B2uspto-grants-2003_12