HRID1806192
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
200 ml of xylene were added to 5-bromoacenaphthylene (14.5 g, 62.8 mmol) and diphenylisobenzofuran (17.1 g, 63.3 mmol) and the mixture was stirred under reflux of xylene for 5 hours. After the mixture was cooled to room temperature, the solvent was distilled off. Then, 26 ml of trifluoroacetic anhydride and 260 ml of chloroform were added thereto, followed by stirring under reflux for 1 hour. After the mixture was cooled to room temperature, the solvent was distilled off. The obtained residue was purified by silica gel chromatography (mobile phase; toluene:heptane=1:3), whereby 16 g of 4-bromo-7,12-diphenylbenzo[k]fluoranthene were obtained as a yellow solid.
WORKUP
后处理
- distillationthe solvent was distilled off
- additionThen, 26 ml of trifluoroacetic anhydride and 260 ml of chloroform were added
- stirringby stirring
- temperatureunder reflux for 1 hour
- temperatureAfter the mixture was cooled to room temperature
- distillationthe solvent was distilled off
- customThe obtained residue was purified by silica gel chromatography (mobile phase; toluene:heptane=1:3)