تفاعل #1726665
ord-e5b9ffe24bfb4755865481d8a016576f
معادلة التفاعل
ظروف التفاعل
المعالجة
- 1أخرىInto a 50 mL three-neck flask were put
- 2أخرىThis mixture was degassed under reduced pressure
- 3ترشيحThen, the mixture was subjected to suction filtration through Florisil (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 540-00135), Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855), and alumina
- 4غسيلThe obtained filtrate was washed with water
- 5تجفيفa saturated saline, and then dried with magnesium sulfate
- 6ترشيحfiltered
- 7تركيزthe obtained filtrate was concentrated
- 8أخرىto give a solid
- 9أخرىThe obtained solid was recrystallized with chloroform/hexane
الإجراء التجريبي
Into a 50 mL three-neck flask were put 1.0 g (2.63 mmol) of 9-iodo-10-phenylanthracene and 542 mg (2.70 mmol) of p-bromophenyl boronic acid. The atmosphere in the flask was replaced with nitrogen. After that, 10 mL of toluene and 3 mL of potassium carbonate aqueous solution (2.0 M) were added to the flask. This mixture was degassed under reduced pressure, then 46 mg (0.03 mmol) of tetrakis(triphenylphosphine)palladium(0) was added to the mixture. The mixture was stirred under a nitrogen stream at 80° C. for 9 hours. After the stirring, about 20 mL of toluene was added to this mixture. Then, the mixture was subjected to suction filtration through Florisil (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 540-00135), Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855), and alumina. The obtained filtrate was washed with water and a saturated saline, and then dried with magnesium sulfate. This mixture was gravity filtered, and the obtained filtrate was concentrated to give a solid. The obtained solid was recrystallized with chloroform/hexane to give 0.56 g of a light-brown solid, which was the object of the synthesis, in a yield of 45%.