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noleg

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zehuac(金币+2):先鼓励一下，谢谢参与啦 2010-06-14 08:34:22
caikedi(金币+30, 翻译EPI+1):谢谢 2010-06-14 09:36:17
In a 250-mL, three-necked, round-bottomed flask equipped with a mechanical stirrer, is placed a calpis consisting of 1,4-dibromobutane(0.1mol), sodium hydroxide(0.1mol) and de-ionized water(100mL). Tetrahydropyrrole is added dropwise at room temperature. The mixture is heated to reflux for 5h. The reaction mixture is then vaporized by reduced pressure distillation. The residue was dilute by isopropanol, filtrated, and the filtrate is concentrated in vacuo, to give crude spirocyclic tetramethyleneammonium bromide. After that, tetrafluoroboric acid(30mL,40%) was added to the residue. The mixture is then distilled in vacuo untill there is no liquid to com out. The residue is allowed to cool down, and is recrystallized twice from absoluted ethanol.

[ Last edited by noleg on 2010-6-14 at 08:45 ]
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