HRID11194
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
5 g (18.5 mmol) of diphenylisobenzofuran and 4.3 g (18.5 mmol) of 5-bromoacenaphthylene in toluene were agitated for 24 hours at the reflux temperature. The solvent was distilled off in vacuum, after which the residue was dissolved in 500 ml of acetic acid. An aqueous 40% hydrobromic acid solution, 50 cm3, was added to the solution, which was heated at 80° C. for one hour. After cooling to room temperature, the precipitate was collected by filtration. This was purified by silica gel chromatography using a mixture of toluene and hexane as an extracting solvent, yielding 7 g of 3-bromo-7,12-diphenylbenzo[k]fluoranthene having a yellowish white color.
WORKUP
后处理
- distillationThe solvent was distilled off in vacuum
- dissolutionafter which the residue was dissolved in 500 ml of acetic acid
- additionAn aqueous 40% hydrobromic acid solution, 50 cm3, was added to the solution, which
- temperatureAfter cooling to room temperature
- filtrationthe precipitate was collected by filtration
- customThis was purified by silica gel chromatography
- additiona mixture of toluene and hexane as an extracting solvent