Reaktion #69945

ord-d4c209656121418b9e37ee965c078d8b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturat reflux for 5 hours
  3. 3
    SonstigeThe reaction mixture is evaporated to dryness The crude product
  4. 4
    Sonstigeis purified by flash chromatography on silica gel

Vorschrift

To a solution of 1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (3 g, 16.6 mmol) in chloroform (8 ml) is added PCl5 portionwise. The reaction mixture is stirred and heated at reflux for 5 hours. The reaction mixture is evaporated to dryness The crude product is purified by flash chromatography on silica gel to give 5-chloro-1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (1.39 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530667B2uspto-grants-2013_09