小白救助,酰胺合成
我是用5-氨基喹啉和苯甲酰氯合成酰胺,下面是合成方法,但是每次都不成功,酰氯也是買的新的,大家知道為什么嗎?求助
Add benzoyl chloride (1.05 equiv) dropwise to a stirred solution of 8-aminoquinoline (1 equiv) and Et3N (1.05 equiv) in anhydrous DCM (0.3 M) under argon at 0 °C.
Stir the resulting solution overnight at room temperature.
Dilute the reaction mixture with DCM.
Wash twice with water, twice with saturated aqueous NaHCO3 and then with brine.
Dry the organic layer over anhydrous Na2SO4 and concentrate under reduced pressure.
Purify the residue by column chromatography on silica gel, eluted with Cyclohexane/EtOAc (from [95:5] to [80:20]).
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昂,是液體的,苯甲酰氯,新買了一瓶沒問題的,謝謝老板這么細(xì)心
重新做了一個(gè),一點(diǎn)反應(yīng)沒有,新點(diǎn)就是酰氯的衍生物
用別的胺檢測一下先氯的質(zhì)量,另外可以投個(gè)常規(guī)的縮合試試
這個(gè)應(yīng)該很簡單,但是如你所說,沒有反應(yīng)的話?紤]原料有問題, 我覺得可能是5-氨基喹啉有問題, 是不是這個(gè)東西是就含有結(jié)晶水的?
反應(yīng)溶劑是啥?加沒有加縛酸劑?