Reaktion #69513

ord-e0b3177f9ddd4c4a82de19eb17756366

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
  2. 2
    workup.STIRRINGAfter thoroughly shaking the mixture
  3. 3
    Sonstigethe organic layer was separated
  4. 4
    Waschenthe organic layer was washed with brine
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    FiltrationThe mixture was then filtered
  7. 7
    workup.DISTILLATIONthe solvent in the filtrate was then distilled off under reduced pressure

Vorschrift

To a dichloromethane (30 mL) mixture of 3-methoxy-1-butanol (3.12 g, 30.0 mmol) and triethylamine (4.62 mL, 33.0 mmol), was added methanesulfonyl chloride (4.62 mL, 33.0 mmol) while stirring on ice, and the mixture was stirred at room temperature for 30 minutes. To the mixture, were added water and ethyl acetate. After thoroughly shaking the mixture, the organic layer was separated, and the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The mixture was then filtered, and the solvent in the filtrate was then distilled off under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530504B2uspto-grants-2013_09