Reaktion #51242

ord-ab789f9d1df541f2bbe68664d376d405

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Trocknenthe organic layer was dried over anhydrous sodium sulfate
  2. 2
    Einengenconcentrated
  3. 3
    Sonstigethe residue was purified by chromatography
  4. 4
    Sonstigeto afford a colorless oil

Vorschrift

To a solution of sodium hydride in 40 mL DMF stirred at 0° C. was slowly added ethyl glycolate (5 g, 48 mmol). After 1 hour, 1,4-dibromobutane (8.6 mL, 72 mmol) was added, and the mixture was stirred for an additional 2 hours. The reaction was allowed to warm to room temperature for an additional 3 hours. A sodium bicarbonate solution was added, and the organic layer was dried over anhydrous sodium sulfate, concentrated and the residue was purified by chromatography to afford a colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06849657B2uspto-grants-2005_02