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yhc0316

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Other 9,9-dialkylfiuorene-carbaldehyde intermediates were synthesized as described for 9,9-didodecylfluorene-2-carbaldehyde except that different 1-alkylbromides were used. After purification, they were used without characterization.
9,10-Bis[(9,9-didodecylfluorene-2-yl)vinyl]anthracene (FLAC12). 9,9-Didodecylfluorene-2-carbaldehyde (0.167 g, 0.46 mmol) and 9,10-bis(diethylphosphorylmethyl)anthracene (0.10 g, 0.21 mmol) were dissolved in 20 mL of anhydrous THF. Potassium tert-butoxide (0.19 g, 1.67 mmol) was added and the resulting suspension was stirred for 5 h at room temperature.  Methanol was added into the mixture and the resulting solid was collected by  filtration. The crude product was purified by silica gel column chromatography (petroleum ether/dichloromethane ¼ 4/1, v/v). After recrystallization from chloroform– methanol, a yellowish-green solid was obtained (0.19 g, 75% yield).
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yhc0316: 金币+30, 翻译EPI+1 2014-10-20 13:44:45
其它9,9 - 二烷基甲醛中间体的合成与9,9 - 二 - 十二烷基芴-2 - 甲醛相同,除了所用的的1 - 烷基溴化物不同。纯化后,无需鉴定便可使用。

9,10 - 双[(9,9 - 二 - 十二烷基芴-2 - 基)乙烯基]蒽(FLAC12)。 9,9 - 二 - 十二烷基芴-2 - 甲醛(0.167克,0.46毫摩尔)和9,10 - 双(二乙基磷酰基)蒽(0.10克,0.21毫摩尔)溶解在20mL无水THF中。加入叔丁醇钾(0.19克,1.67毫摩尔)后将得到的悬浮液在室温下搅拌5小时。将甲醇溶液中加入到混合物中,将所得固体通过过滤收集。将粗产物用硅胶柱层析法纯化(石油醚/二氯甲烷=4:1,体积/体积)。从氯仿 - 甲醇中重结晶后,得到黄绿色固体(0.19克,75%产率)。
2楼2014-10-20 08:43:45
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