Reaktion #659893

ord-f87d7ae9aaa0481cb8a4d9ee5db5f77a

Lösungsmittel

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeReaction
  2. 2
    Temperaturwas cooled
  3. 3
    WaschenOrganic layer was washed 4 times at 70° C
  4. 4
    SonstigeToluene removed

Vorschrift

To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), TMPD glycol (146.2 g, 1.0 moles) and potassium carbonate (73 g, 0.53 moles). The mixture was heated to 120° C. and held for 4 hours. Reaction was cooled and 200 mL of toluene added. Organic layer was washed 4 times at 70° C. Toluene removed to provide 275 g of product. GC assay of the product was 95.9% (4.6:1 mixture of two major isomers).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09029451B2uspto-grants-2015_05