Reaktion #69565

Reaktionsgleichung

7,7′-dibromo-3,3′,5,5′-tetramethyl-1,1′-biadamantane

1,3-dibromo benzene

aluminum bromide

→

7,7′-bis(3,5-dibromophenyl)-3,3′,5,5′-tetramethyl-1,1′-biadamantane

Ausbeute 180.0%

Lösungsmittel

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA 3-liter recovery flask was charged with the
2. 2
   workup.ADDITIONAfter the end of addition
3. 3
   workup.STIRRINGthe solution was stirred at 50° C. for 7 hours
4. 4
   Sonstigethe aqueous phase was removed by separation
5. 5
   workup.ADDITIONacetone 1 liter was added for extraction
6. 6
   FiltrationThe solid was collected by filtration
7. 7
   Sonstigedried under reduced pressure

Vorschrift

A 3-liter recovery flask was charged with the above synthesized 7,7′-dibromo-3,3′,5,5′-tetramethyl-1,1′-biadamantane 48.4 g (100 mmol), 1,3-dibromo benzene 1180 g (500 mmol), and a stirrer. While stirring under a nitrogen flow at room temperature, aluminum bromide (III) 26.7 g (100 mmol) was added little by little. After the end of addition, the solution was stirred at 50° C. for 7 hours. The reaction solution was charged into a 1 mol/liter hydrochloric acid solution 2 liter, the aqueous phase was removed by separation, then acetone 1 liter was added for extraction. The solid was collected by filtration and dried under reduced pressure to obtain 7,7′-bis(3,5-dibromophenyl)-3,3′,5,5′-tetramethyl-1,1′-biadamantane (90.0 mmol; yield 90.0%) 71.5 g.

Quelle