تفاعل #1543037
ord-4719ee4de4624803a19d4699cd571b1f
معادلة التفاعل
الكواشف
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المعالجة
- 1أخرىA 200-milliliter 3-necked round bottom flask equipped with a mechanical stirrer
- 2درجة الحرارةreflux condenser, and argon inlet
- 3أخرىwas purged with argon
- 4درجة الحرارةThe mixture was cooled to about 100° C.
- 5أخرىThe resulting two phase mixture was transferred into a separatory funnel
- 6أخرىthe layers separated
- 7غسيلwas washed with water
- 8workup.ADDITIONtreated with 25 grams of alumina under an argon atmosphere
- 9ترشيحfiltered
- 10أخرىThe filtrate was then evaporated
- 11أخرىthe residue was recrystallized from cyclohexane
الإجراء التجريبي
A 200-milliliter 3-necked round bottom flask equipped with a mechanical stirrer, reflux condenser, and argon inlet was purged with argon and then charged with 5,11-dihydroindolo[3,2-b]carbazole (5.1 grams, 0.02 mol), 3-iodotoluene (8.69 grams, 0.04 mol), copper sulfate pentahydrate (0.25 gram, 1.0 mmol), potassium carbonate (5.52 grams, 0.04 mol), and n-tridecane (5.0 milliliters). Under an argon atmosphere, the reaction mixture was heated to about 250° C. with a heating mantle and allowed to proceed at this temperature to completion in about 6 hours. The mixture was cooled to about 100° C., and 100 milliliters of toluene and 15 milliliters of water were then added with vigorous stirring. The resulting two phase mixture was transferred into a separatory funnel and the layers separated. The organic phase, which contained the desired product, was washed with water, and treated with 25 grams of alumina under an argon atmosphere, and filtered. The filtrate was then evaporated and the residue was recrystallized from cyclohexane to provide 6.8 grams of pure, about 99.9 percent, 5,11-di-m-tolyl-5,11-dihydroindolo-[3,2-b]carbazole (1).