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caikedi木虫 (正式写手)
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| 室温搅拌下，于250mL三口烧瓶中，将四氢吡咯（0.1mol）滴入含有1，4-二溴丁烷（0.1mol）、NaOH（0.1mol）和去离子水（100mL）的乳浊液中，加热回流5小时。减压蒸馏，加入异丙醇，过滤，减压浓缩，得到溴代四亚甲基螺环季铵盐粗品，再加入40%四氟硼酸溶液（30mL），然后减压蒸馏至无液体流出，冷却，加入无水乙醇重结晶2次。 |
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noleg
金虫 (小有名气)
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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
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
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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 ] |
3楼2010-06-14 08:30:10
xiaoqihu
铁杆木虫 (著名写手)
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wypward(金币+1):谢谢参与 2010-06-13 15:57:55
zehuac(金币+1):谢谢参与哈，希望以后更加积极的应助 2010-06-16 13:03:47
wypward(金币+1):谢谢参与 2010-06-13 15:57:55
zehuac(金币+1):谢谢参与哈，希望以后更加积极的应助 2010-06-16 13:03:47
| To a stirred mixture of 1,4-Dibromo butane （0.1mol）, sodium hydroxide （0.1mol）and distilled water (100mL) was added tetrahydro pyrrole （0.1mol) at r.t. After addition of tetrahydro pyrrole, the reaction mixture was heated to reflux for 5 hours, the reaction solution, then, was distilled under vacuum. The obtained residue was diluted with isopropanol, filtrated, and the filtrates was concentrated to afford crude 溴代四亚甲基螺环季铵盐. After that, the 四氟硼酸溶液（30mL）was added and distillation to no liquid come out, cooled down to r.t., recrystallated in absoluted ethanol. |
2楼2010-06-13 15:08:19
