反応 #505212

反応方程式

triphenylene

bromine

→

product

収率 69.8%

2-bromotriphenylene

収率 69.8%

溶媒

trim ethyl phosphate

trim ethyl phosphate

反応条件

後処理

1. 1
   その他The reaction was quenched
2. 2
   workup.ADDITIONby pouring into ice water
3. 3
   抽出extracted with dichloromethane
4. 4
   洗浄washed with saturated sodium bisulfate solution
5. 5
   乾燥After drying with magnesium sulfate
6. 6
   その他the solvent was evaporated

実験手順

3.2 g (14 mmol) of triphenylene was dissolved in 60 mL of trim ethyl phosphate. To the suspension was added 2.23 g (14 mmol) of bromine in 10 mL of trim ethyl phosphate at room temperature under N2. The mixture was then heated up to 80° C. The reaction was monitored by HPLC. The reaction was quenched by pouring into ice water, then extracted with dichloromethane and washed with saturated sodium bisulfate solution. After drying with magnesium sulfate, the solvent was evaporated. The crude product was run through a short silica gel plug using dichloromethane. 3.0 g of product was obtained after drying under vacuum. The product contains triphenylene, 1-bromotriphenylene, 2-bromotriphenylene, and a mixture of dibromotriphenylene isomers.

出典