Reaktion #818395
ord-4d9162968f024969a493a6db5ba91605
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2Temperaturat reflux for 16 hours
- 3EinengenThe mixture was concentrated under reduced pressure to about 50 mL
- 4FiltrationThe reaction was then filtered
- 5Waschenthe solid was washed with Et2O (20 mL)
- 6EinengenThe combined organic solution was then concentrated under vacuum
- 7Sonstigeused 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.