反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A 1 M solution of boron tribromide in dichloromethane, (0.55 cm3, 0.00581 mol) was added dropwise to a stirred solution of 9,9-dioctyl-2-(4-nonylphenyl)-7-octyloxyfluorene (2.79 g, 0.00388 mol) and dichloromethane (100 cm3) at 0° C. The temperature was allowed to rise to RT overnight and the solution added to ice-water (200 cm3) with vigorous stirring. The product was extracted into diethyl ether (2×200 cm3). The combined organic extracts were washed with saturated aqueous sodium carbonate solution (150 cm3), dried (MgSO4), filtered and the solvent removed under reduced pressure. The residue was purified by column chromatography [silica gel, dichloromethane:hexane: 20:80] (yield 2.2 g, 93.4%).
WORKUP
后处理
- extractionThe product was extracted into diethyl ether (2×200 cm3)
- washThe combined organic extracts were washed with saturated aqueous sodium carbonate solution (150 cm3)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customthe solvent removed under reduced pressure
- customThe residue was purified by column chromatography [silica gel, dichloromethane:hexane: 20:80] (yield 2.2 g, 93.4%)