Reaktion #7363

ord-e695220a42e7464caba10ab706dbb1bd

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a 1.5 L autoclave equipped with a stirrer
  2. 2
    Sonstigewas sealed
  3. 3
    TemperaturThen the reaction mixture was cooled to room temperature
  4. 4
    Sonstigedischarged into a 1 L three-necked flask
  5. 5
    TemperaturThe reaction mixture was heated to 45° C. for 4 h
  6. 6
    workup.STIRRINGwhile stirring
  7. 7
    FiltrationAfter filtration, part of ethanol
  8. 8
    workup.DISTILLATIONwas distilled off from the filtrate
  9. 9
    workup.ADDITIONThen 500 g of water was added while ethanol
  10. 10
    workup.DISTILLATIONwas distilled off (part of water was entrained out)

Vorschrift

To a 1.5 L autoclave equipped with a stirrer and a heating means were added 154 g (1.0 mol) of diethyl sulfate, 101 g (1.0 mol) of triethyl amine and 690 g (15 mol) of ethanol. Stirring was initiated after the autoclave was sealed. The autoclave was heat to 140° C., and pressure was 1.0 MPa. The reaction was kept at 140° C. for 4 h. Then the reaction mixture was cooled to room temperature and discharged into a 1 L three-necked flask. 80 g (2.0 mol) of sodium hydroxide was added thereto. The reaction mixture was heated to 45° C. for 4 h while stirring. After filtration, part of ethanol was distilled off from the filtrate. Then 500 g of water was added while ethanol was distilled off (part of water was entrained out), to give 604 g of tetraethyl ammonium hydroxide solution. The content of tetraethyl ammonium hydroxide was found as 23.3 wt.-% and the total reaction yield was 95.7%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084302B2uspto-grants-2006_08