반응 #2016150
ord-b05e134d621c4048906f8102304dc317
반응 방정식
반응 조건
후처리
- 1workup.ADDITIONwas dropped in the reaction solution at the room temperature
- 2workup.STIRRINGthe solution was further stirred for 1 hour
- 3세척An organic layer of the reaction mixture was washed with aqueous sodium hydroxide (2.0 mol/L) and saturated saline
- 4건조dried with magnesium sulfate
- 5여과This mixture was filtrated naturally
- 6기타condensed
- 7기타to obtain a solid
- 8여과the solution was subjected to suction filtration through Florisil, celite
- 9농축The filtrate was concentrated
- 10기타to obtain a solid
- 11기타the solid was recrystallized with a mixture solution of dichloromethane and hexane, whereby 27.8 g of a light yellow powdery solid
- 12기타was obtained with the yield of 85%
실험 절차
25.0 g (98.3 mmol) of 9-phenylanthracene was put into a 1-L three-neck flask, and 300 mL of carbon tetrachloride was added thereto. A solution in which 15.6 g (98.3 mmol) of bromine was dissolved in 40 mL of carbon tetrachloride was dropped in the reaction solution at the room temperature. After the dropping, the reaction solution was stirred at the room temperature for 1 hour. Thereafter, the reaction is completed by adding a sodium thiosulfate aqueous solution, and the solution was further stirred for 1 hour. An organic layer of the reaction mixture was washed with aqueous sodium hydroxide (2.0 mol/L) and saturated saline and dried with magnesium sulfate. This mixture was filtrated naturally, and the filtrate was condensed to obtain a solid. The solid was dissolved in toluene, and the solution was subjected to suction filtration through Florisil, celite, and then alumina. The filtrate was concentrated to obtain a solid, and the solid was recrystallized with a mixture solution of dichloromethane and hexane, whereby 27.8 g of a light yellow powdery solid that was a target matter was obtained with the yield of 85%.