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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沒有人知道為啥沒反應(yīng)嗎...
賂脨戮玫虜?shù)擉H脡脨脨
做過好幾種酰胺都是酰氯與胺在甲苯下回流就能完成
脦脪脪虜脳枚鹿媒潞脙錄賂脰脰脕脣攏盧脙驢脰脰路陸路簍露錄虜?shù)撁挼撁懨箶n盧驢脡脛脺祿祿脤氓脧碌戮脥脮芒賂枚路陸路簍虜?shù)撀好兠撁兠伱嫈n盧脳枚脮芒賂枚脠脣潞脺脡脵賂脨戮玫隆?br>,
是一點(diǎn)兒都沒轉(zhuǎn)化還是收率低呀?
賂脨戮玫脪祿碌茫露錄脙祿路麓脫婁....tcl碌茫擄氓脢脟3賂枚碌茫攏盧2賂枚脭顱脕脧隆攏脝盲脰脨脪祿賂枚驢脡脛脺脢脟玫攏脗脠碌脛脩脺脡煤脦茂