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1 ,1 '-Dibromoferrocene (0.67 g, 1.97 mmol) in anhydrous tetrahydrofuran (THF) (30 ml) was placed in a reaction vessel and cooled to -78 0C using a dry ice and acetone mixture, n-butyl lithium (0.94 ml, 2.36 mmol) was added under inert conditions thereto and the contents of the reaction vessel kept stirred for approximately 1 hour while cold zinc chloride (2.16 ml, 2.16 mmol) was added. Tetrakis(triphenylphosphine)palladiumO (50 mg) and 4,5- dichlorophthalonitrile (0.5 g, 1.97 mmol) were then added. The contents of the reaction vessel were allowed to warm to room temperature and were kept stirred for approximately 2 hours before heating to approximately 90 0C for 12 hours. Thereafter, water (20 ml) was added and extracted with dichloromethane (3 x 20 ml). The combined organic layers were dried over magnesium sulfate and reduced to dryness under reduced pressure to obtain a crude product. The crude product was placed on alumina and eluted with diethyl ether ; petroleum spirit (55:45) to yield red crystals.
1 ,1'-Dibromoferrocene (0.67 g, 1.97 mmol) in anhydrous tetrahydrofuran (THF) (30 ml) was placed in a reaction vessel and cooled to -78 0C using a dry ice and acetone mixture, ?-butyl lithium (0.94 ml, 2.36 mmol) was added under inert conditions thereto and the contents of the reaction vessel kept stirred for approximately 1 hour while cold zinc chloride (2.16 ml, 2.16 mmol) was added. Tetrakis(triphenylphosphine)palladiumO (50 mg) and 4,5- dichlorophthalonitrile (0.5 g, 1.97 mmol) were then added. The contents of the reaction vessel were allowed to warm to room temperature and were kept stirred for approximately 2 hours before heating to approximately 90 C for 12 hours. Thereafter, water (20 ml) was added and extracted with dichloromethane (3 x 20 ml). The combined organic layers were dried over magnesium sulfate and reduced to dryness under reduced pressure to obtain a crude product. The crude product was placed on alumina and eluted with diethyl ether ; petroleum spirit (55:45) to yield red crystals.
ethyl 4-(2-chloro-4,5-dicyanophenoxy)-3-methoxybenzoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With potassium carbonate; In N,N-dimethyl-formamide; at 100℃; for 12h;Inert atmosphere;
4,5-dichlorophthalonitrile (5.0 mmol), <strong>[617-05-0]ethyl vanillate</strong> (7.5 mmol) and K2CO3 (50.0 mmol) were dissolved in 30 ml of anhydrous DMF under a nitrogen gas atmosphere And refluxed at 100 [deg.] C for 12 hours When the reaction was complete, the reaction solution was slowly added dropwise to ice-water. The precipitate was filtered under reduced pressure, washed with distilled water, The dried crude product was purified by column chromatography (eluent: MC = 100%).
With potassium carbonate; In N,N-dimethyl-formamide; at 100℃; for 12h;Inert atmosphere;
Under nitrogen gas, 4,5-dichlorophthalonitrile (5.0 mmol), <strong>[617-05-0]ethyl vanillate</strong> (7.5 mmol), K2CO3 (50.0 mmol) was dissolved in 30 ml of anhydrous DMF and refluxed at 100 for 12 hours. When the reaction was complete, the reaction solution was slowly dropped on ice-water in a dropwise manner. The precipitate was filtered under reduced pressure, washed with distilled water, The dried crude product was purified by column chromatography (eluent: MC: MeOH = 15: 1).
With potassium carbonate; In N,N-dimethyl-formamide; at 100℃; for 12h;Inert atmosphere;
Under nitrogen gas, 4,5-dichlorophthalonitrile (5.0 mmol),Ethyl vanillate (7.5 mmol), K2CO3 (50.0 mmol) was dissolved in 30 ml of anhydrous DMF and refluxed at 100 for 12 hours.When the reaction was complete, the reaction solution was slowly dropped on ice-water in a dropwise manner. The precipitate was filtered under reduced pressure, washed with distilled water,The dried crude product was purified by column chromatography (eluent: MC: MeOH = 15: 1).
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