반응 #505212

반응 방정식

triphenylene

bromine

→

product

수율 69.8%

2-bromotriphenylene

수율 69.8%

용매

trim ethyl phosphate

trim ethyl phosphate

반응 조건

후처리

1. 1
   기타The reaction was quenched
2. 2
   workup.ADDITIONby pouring into ice water
3. 3
   추출extracted with dichloromethane
4. 4
   세척washed with saturated sodium bisulfate solution
5. 5
   건조After drying with magnesium sulfate
6. 6
   기타the solvent was evaporated

실험 절차

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.

출처