重氮對苯(酉昆)(p-Diazobenzoquinone)的創新製備方法是:將重氮對酚氫硫酸鹽(p-Phenoldiazonium hydrogen sulfate)溶於無水甲醇(CH3OH),冰浴下攪拌,再加入氧化鈣(CaO),反應完成後將溶液過濾,取濾液進行乾式管柱層析分離(Alumina gel),可得到淡黃色液體,經減壓濃縮機濃縮,得到產物重氮對苯(酉昆)。在未進行乾式管柱層析分離(Alumina gel)前,濾液在冰箱冷藏一段時間,意外地發現中間物晶體。 本論文的研究目的是以X-ray單晶繞射儀來解中間物晶體的構造,以瞭解中間物到底是什麼?並利用重氮對苯(酉昆)的創新製備方法,製備重氮對苯(酉昆)的類似物重氮奈(酉昆)(Diazonaphthoquinone)。
A novel method to synthesize p-Diazobenzoquinone is reported in this thesis. The protocol is dissolving p-Phenoldiazonium hydrogen sulfate in absolute methanol and adding calcium oxide. This mixture is stirred and kept at 0℃ for 3hr. The solution is then filtered. The filtrate passing through a short alumina gel column give light yellow elusion which is then evaporated to give the product p-Diazobenzoquinone. If not passing through a short alumina gel column the filtrate give a crystal while keeping in a refrigerator for a period of time. The purpose of this project is to find out what the crystal is by X-ray diffraction and utilize the novel method to synthesize diazonaphthoquinone.
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