Reaktion #214262

ord-43d41b4cfe194fcd806cb95b242b0ecf

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter the resulting exothermic reaction
  2. 2
    Temperaturis heated at 130° C. for one hour
  3. 3
    workup.DISTILLATIONThe crude product is evaporatively distilled
  4. 4
    Sonstigeto give a liquid, pmr spectrum (CDCl3)

Vorschrift

A stirred mixture of 23.8 g of 4-cyclopropyl-4-trimethylsiloxy-1-octyne (Example 191), 28 ml of tri-n-butyltin hydride, and 50 mg of azobisisobutyronitrile under nitrogen is heated to 85° C. After the resulting exothermic reaction subsides the mixture is heated at 130° C. for one hour. The crude product is evaporatively distilled to give a liquid, pmr spectrum (CDCl3): δ0.10 (trimethylsiloxy group), 2.33 (doublet, =CHCH2), and 6.02 (vinyl hydrogens).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04254285uspto-grants-1981_03