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| 室溫攪拌下，于250mL三口燒瓶中，將四氫吡咯（0.1mol）滴入含有1，4-二溴丁烷（0.1mol）、NaOH（0.1mol）和去離子水（100mL）的乳濁液中，加熱回流5小時。減壓蒸餾，加入異丙醇，過濾，減壓濃縮，得到溴代四亞甲基螺環(huán)季銨鹽粗品，再加入40%四氟硼酸溶液（30mL），然后減壓蒸餾至無液體流出，冷卻，加入無水乙醇重結(jié)晶2次。 |
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xiaoqihu
鐵桿木蟲 (著名寫手)
- 翻譯EPI: 88
- 應(yīng)助: 1 (幼兒園)
- 貴賓: 0.005
- 金幣: 9724.8
- 散金: 7
- 紅花: 4
- 帖子: 1337
- 在線: 105.6小時
- 蟲號: 590066
- 注冊: 2008-08-31
- 專業(yè): 有機合成
★ ★
wypward(金幣+1):謝謝參與 2010-06-13 15:57:55
zehuac(金幣+1):謝謝參與哈，希望以后更加積極的應(yīng)助 2010-06-16 13:03:47
wypward(金幣+1):謝謝參與 2010-06-13 15:57:55
zehuac(金幣+1):謝謝參與哈，希望以后更加積極的應(yīng)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 溴代四亞甲基螺環(huán)季銨鹽. 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樓2010-06-13 15:08:19
noleg
金蟲 (小有名氣)
- 翻譯EPI: 52
- 應(yīng)助: 0 (幼兒園)
- 貴賓: 0.005
- 金幣: 1423.7
- 帖子: 161
- 在線: 43.9小時
- 蟲號: 932452
- 注冊: 2009-12-23
- 性別: GG
★ ★
zehuac(金幣+2):先鼓勵一下，謝謝參與啦 2010-06-14 08:34:22
caikedi(金幣+30, 翻譯EPI+1):謝謝 2010-06-14 09:36:17
zehuac(金幣+2):先鼓勵一下，謝謝參與啦 2010-06-14 08:34:22
caikedi(金幣+30, 翻譯EPI+1):謝謝 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樓2010-06-14 08:30:10
zhangbo2706
木蟲 (著名寫手)
- 應(yīng)助: 17 (小學(xué)生)
- 金幣: 4300.4
- 散金: 64
- 紅花: 2
- 沙發(fā): 2
- 帖子: 1953
- 在線: 1333.8小時
- 蟲號: 1008673
- 注冊: 2010-04-29
- 性別: GG
- 專業(yè): 其他無機非金屬材料
4樓2010-06-14 09:13:23
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