Reaktion #1196451

ord-b5ee72f5d3f34620ab6e00580639cac8

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas cooled in a water bath
  2. 2
    Sonstigeexcess thionyl chloride was removed by distillation
  3. 3
    workup.DISTILLATIONthe crude acid was then fractionally distilled

Vorschrift

2,2-dimethyl valeric acid (49.0 g, 377 mmol) was added dropwise over 1 hour with stirring to freshly distilled thionyl chloride (102 g, 860 mmol) that was cooled in a water bath. After stirring for an additional 1/2 hour in a warm water bath, excess thionyl chloride was removed by distillation and the crude acid was then fractionally distilled to give 49.7 g of product that assayed >95% by gas chromatography, bp 45°/10.5 mm (lit. bp 45°/10 mm).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05319133uspto-grants-1994_06