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書(shū)劍如風(fēng)新蟲(chóng) (著名寫(xiě)手)
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| 將碳酸鉀, 氧化銅和二苯胺于研缽中研勻后加入到50ml圓底燒瓶中，加熱至體系內(nèi)的二苯胺熔化，攪拌下反應(yīng)2h后停止加熱，冷卻，將瓶?jī)?nèi)固體溶于二氯甲烷,并用適量硅膠吸附后蒸干，依次用EtOAc/ CH2Cl2=1:8, EtOAc/ CH2Cl2 =1:18柱層析分離得淺褐色固體，再將其溶解于氯仿,加入適量活性炭脫色，過(guò)濾，旋蒸濃縮得白色固體。 |
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書(shū)劍如風(fēng): 金幣+80, 翻譯EPI+1 2015-09-15 06:59:06
書(shū)劍如風(fēng): 金幣+80, 翻譯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樓2015-09-14 22:33:55
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