Reaktion #945454

ord-592b54ede64b4dbb8ac5bfcd345c18b3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with dichloromethane
  2. 2
    Waschenwashed with water
  3. 3
    Sonstigethe organic phase is separated out after settling
  4. 4
    Trocknendried over magnesium sulphate
  5. 5
    Sonstigeevaporated
  6. 6
    SonstigeAfter recrystallization of the residue from methanol, 17.78 g (63%) of the expected compound
  7. 7
    Sonstigeare collected in the form of fine white crystals with a melting point of 73° C.

Vorschrift

18.31 g (100.0 mmol) of 2,5-dichloro-2,5-dimethylhexane, 17.10 g (100.0 mmol) of 2-bromotoluene and 200 ml of 1,2-dichloroethane are introduced into a three-necked flask under an argon atmosphere. 1.33 g (10.0 mmol) of aluminium chloride are added rapidly in a single portion and the reaction medium is stirred for thirty minutes at room temperature. The reaction medium is poured into water, extracted with dichloromethane and washed with water, and the organic phase is separated out after settling has taken place, dried over magnesium sulphate and evaporated. After recrystallization of the residue from methanol, 17.78 g (63%) of the expected compound are collected in the form of fine white crystals with a melting point of 73° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07148245B2uspto-grants-2006_12