Reaktion #1248537

ord-3677f50506fc4935bf76f6977304ac04

Lösungsmittel

Reaktionsbedingungen

Temperatur
2.5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 2.5 h
  2. 2
    TemperaturThe mixture was then refluxed for 2 h
  3. 3
    Temperaturcooled to room temperature
  4. 4
    Filtrationthe white solid filtered off
  5. 5
    Waschenwashed with ether

Vorschrift

15.9 g (81 mmol) of 7-Bromo-bicyclo[2.2.1]heptane were added dropwise to 2 g magnesium (81 mmol) in 25 ml of diethyl ether and refluxed for 2.5 h. The mixture was cooled to 0-5° C. and 6.3 ml (81 mmol) of DMF were added dropwise. The mixture was then refluxed for 2 h, cooled to room temperature and the white solid filtered off and washed with ether. The filtrate was reduced and 4.87 g of a white solid were obtained. The intermediate was used without further characterization.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07816540B2uspto-grants-2010_10