반응 #2421
ord-76651472f2d84918bce8909e6a061689
반응 방정식
반응물
반응 조건
후처리
- 1기타A 1 L, three-necked, round-bottomed flask, equipped with an overhead stirrer, a nitrogen inlet and a reflux condenser
- 2기타With a slow purge of nitrogen through the condenser
- 3기타the reaction vessel was placed in an oil bath
- 4기타the stirred reaction
- 5여과The hot reaction mixture was filtered through a bed
- 6여과of filtering aid, which
- 7세척was washed with toluene (50 mL)
- 8농축the filtrate was concentrated on a rotavapor under reduced pressure
- 9기타The solvent residue was further removed with a Kugelrohr apparatus
- 10기타to afford a dark brown viscous oil
실험 절차
A 1 L, three-necked, round-bottomed flask, equipped with an overhead stirrer, a nitrogen inlet and a reflux condenser, was charged with N,N'-diphenyl-1,4-phenylenediamine (13.0 g, 0.05 mol), 4-iodochlorobenzene (31.0 g, 0.13 mol), copper bronze powder (12.7 g, 0.20 mol), 18-crown-6 ether (2.6 g, 0.10 mol), powdered potassium carbonate (50.1 g. 0.36 mol) and 1,2-dichlorobenzene (120 mL). With a slow purge of nitrogen through the condenser, the reaction vessel was placed in an oil bath and the stirred reaction was heated at 200° C. for 20 hours. The hot reaction mixture was filtered through a bed of filtering aid, which was washed with toluene (50 mL), and the filtrate was concentrated on a rotavapor under reduced pressure. The solvent residue was further removed with a Kugelrohr apparatus to afford a dark brown viscous oil. Flash chromatography on a silica gel column (5×25 cm, 5% CH2Cl2 in hexane as eluent) afforded 9.6 g of grey-white solid. The crude product was further washed with toluene and acetone to provide 6.1 g (25%) of off-white powdered material. The polymer of this example is useful for hole transport materials in light-emitting diode devices.