反应 #1904044
ord-e0963ecf552c407d8e4654c0f33da8c9
反应方程式
反应条件
后处理
- 1温度refluxed
- 2温度heated
- 3workup.STIRRINGunder stirring at 60° C.
- 4过滤insoluble matter was filtered off
- 5其他dried
- 6workup.ADDITIONHexane was added to the residue
- 7过滤was filtered off
- 8其他condensed
- 9其他recrystallized with a mixed solvent of hexane/ethyl acetate
实验过程
50.0 g (177 mmole) of 4-bromoiodobenzene, 28.5 g (177 mmole) of 2-phenylindole, 30.5 g (221 mmole) of potassium carbonate, 18.7 g of copper powder, and 150 ml of o-dichlorobenzene were put in a 500 ml three-necked flask, and refluxed with stirring for 25 hours under nitrogen flow. Toluene was added to the reaction mixture heated under stirring at 60° C., and insoluble matter was filtered off. The filtrate was vacuum dried. Hexane was added to the residue and deposited crystal was filtered off. The filtrate was condensed, and refined by silica gel column chromatography (eluent:hexane/ethyl acetate: 50/1), recrystallized with a mixed solvent of hexane/ethyl acetate to give 25.7 g of a white crystal of 1-(4-bromophenyl)-2-phenylindole (yield: 50.1%).