Reaktionsgleichung
Br[C:2]12[CH2:24][C:6]3([CH3:25])[CH2:7][C:8]([C:11]45[CH2:21][C:15]6([CH3:22])[CH2:16][C:17](Br)([CH2:19][C:13]([CH3:23])([CH2:14]6)[CH2:12]4)[CH2:18]5)([CH2:10][C:4]([CH3:26])([CH2:5]3)[CH2:3]1)[CH2:9]2.Br[C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([Br:34])[CH:29]=1.[Br-:35].[Al+3].[Br-:37].[Br-:38].Cl>>[Br:35][C:2]1[CH:3]=[C:4]([C:2]23[CH2:3][C:4]4([CH3:26])[CH2:10][C:8]([C:11]56[CH2:21][C:15]7([CH3:22])[CH2:16][C:17]([C:28]8[CH:33]=[C:32]([Br:38])[CH:31]=[C:30]([Br:34])[CH:29]=8)([CH2:19][C:13]([CH3:23])([CH2:14]7)[CH2:12]5)[CH2:18]6)([CH2:7][C:6]([CH3:25])([CH2:5]4)[CH2:24]2)[CH2:9]3)[CH:5]=[C:6]([Br:37])[CH:24]=1Komponenten
Versuchsvorschrift
In a 1 L recovery flask, 48.4 g of 7,7′-dibromo-3,3′,5,5′-tetramethyl-1,1′-biadamantane (100 mmol), 1,180 g of 1,3-dibromobenzene (5.00 mol) and a stirrer were charged. Under nitrogen flow, 26.7 g of aluminum bromide (100 mmol) was gradually added thereto with agitating at room temperature. After the addition, the mixture was agitated at 50° C. for seven hours. Reaction solution was added to 2 L of 1 mol/L hydrochloric acid aqueous solution. After an aqueous layer was separated and removed therefrom, 1 L of acetone was added. Solid thus precipitated was collected by filtration and dried under reduced pressure, thus obtaining 71.5 g of 7,7′-bis(3,5-dibromophenyl)-3,3′,5,5′-tetramethyl-1,1′-biadamantane (90.0 mmol; yield: 90.0%).
Aufarbeitung
- additionAfter the addition
- stirringthe mixture was agitated at 50° C. for seven hours
- customReaction solution
- customAfter an aqueous layer was separated
- customremoved
- addition1 L of acetone was added
- customSolid thus precipitated
- filtrationwas collected by filtration
- customdried under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-a5434d3484454dacb04ccc5387732d5c
- Quelldatensatz
- uspto-grants-2011_01
- Patentnummer
- US07863347B2
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