重氮對苯(酉昆)之創新製備

The Novel Preparation of p-Diazobenzoquinone

陳冠州(Kuan-Chou Chen)

指導教授 ： 楊嘉喜

中原大學/理學院/化學研究所/碩士(2001年)

https://doi.org/10.6840/cycu200100293

摘要

研究的目的是以創新的合成方式來製備重氮對苯(酉昆)(p-Diazobenzoquinone)。化合物的合成方式是：將重氮對氨基酚氫硫酸鹽(p-Diazophenol hydrogen sulfate)溶於無水甲醇(CH3OH)中，冰浴下攪拌，再加入氧化鈣(CaO)，反應完成之後將溶液過濾，取濾液進行乾式管柱層析分離(Aluminum Gel)，可得到淡黃色液體粗產物，再經減壓濃縮機濃縮，可得到淡黃色油狀物，再加入適量的乙醚(Ether)冷藏逼晶，最後得到產物(橘黃色針狀晶體) 重氮對苯(酉昆)(p-Diazobenzoquinone)。在未進行乾式管柱層析分離(Aluminum Gel)前，濾液在冰箱冷藏一段時間，意外地發現中間物，化合物是以晶體的結構存在，根據元素分析儀的測試結果，可得知是帶有NN雙鍵的化合物，分子量大約是194，其結構式尚未定義。

關鍵字

重氮苯(酉昆) ； 重氮對苯(酉昆) ； 重氮

並列摘要

The purpose of this project is to develop a novel method to synthesize p-Diazobenzoquinone. p-Diazophenol hydrogen sulfate was dissolved in absolute methanol and calcium oxide was added. It was stirred and kept at 0℃ for 3hr. The solution was then filtered. The filtrate was passed through a short aluminum gel column. The light yellow elute was evaporated to an oil. The orange prisms of p-Diazobenzoquinone crystallized in ether at a temperature below 0℃. The filtrate without passing through a short aluminum gel column was accompanied with an crystal intermediate while keeping in a refrigerator for a period of time. But the structure of this intermediate is not yet known.

並列關鍵字

p-Diazobenzoquinone ； benzoquinone ； Diazobenzoquinone

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