Reaktion #818395

ord-4d9162968f024969a493a6db5ba91605

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 16 hours
  3. 3
    EinengenThe mixture was concentrated under reduced pressure to about 50 mL
  4. 4
    FiltrationThe reaction was then filtered
  5. 5
    Waschenthe solid was washed with Et2O (20 mL)
  6. 6
    EinengenThe combined organic solution was then concentrated under vacuum
  7. 7
    Sonstigeused directly in the next step without further purification

Vorschrift

The mixture of 6-bromo-7-methyl-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene (4.20 g, 15 mmol), NBS (3.20 g, 18 mmol), 2,2′-azobisisobutyronitrile (0.3 g, 1.8 mmol) and CCl4 (120 mL) was heated at reflux for 16 hours. The mixture was concentrated under reduced pressure to about 50 mL. The reaction was then filtered, and the solid was washed with Et2O (20 mL). The combined organic solution was then concentrated under vacuum to generate crude product. Crude 91.2 was generated as a brown oil and used directly in the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07582803B2uspto-grants-2009_09