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书剑如风新虫 (著名写手)
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| 将碳酸钾, 氧化铜和二苯胺于研钵中研匀后加入到50ml圆底烧瓶中，加热至体系内的二苯胺熔化，搅拌下反应2h后停止加热，冷却，将瓶内固体溶于二氯甲烷,并用适量硅胶吸附后蒸干，依次用EtOAc/ CH2Cl2=1:8, EtOAc/ CH2Cl2 =1:18柱层析分离得浅褐色固体，再将其溶解于氯仿,加入适量活性炭脱色，过滤，旋蒸浓缩得白色固体。 |
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书剑如风: 金币+80, 翻译EPI+1 2015-09-15 06:59:06
书剑如风: 金币+80, 翻译EPI+1 2015-09-15 06:59:06
| Potassium carbonate, copper oxide and diphenylamine were ground evenly in a mortar and transferred to a 50 ml round bottom flask, heated to melt the diphenylamine in the system and kept stirring for 2 h for the reaction. The reaction was terminated by stop heating and the solid in the flask was dissolved in methylene methane after cooling, evaporated after adsorption with an appropriate amount of silica gel, washed sequentially with EtOAc/CH2Cl2 = 1: 8 and EtOAc/CH2Cl2 = 1: 18. A light brown solid was obtained after column chromatography which was then dissolved in chloroform, decolorized by adding an appropriate amount of active carbon and a white solid was obtained after filtration and concentration by rotary evaporation. |
2楼2015-09-14 22:33:55