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有机反应的后处理实例

2019-07-18 30页 ppt 4MB 39阅读

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有机反应的后处理实例PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt....
有机反应的后处理实例
:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/下载:www.1ppt.com/jiaoan/WorkupofOrganicReactions有机反应的后处理ForIntermalUseOnlyPPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/主要内容 后处理的目的和评价标准 后处理的常规方法2.1不同溶剂的后处理2.2不同底物的后处理2.3特殊试剂的后处理 易燃易爆剧毒品的后处理 后处理常见问题解决方法PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/1.后处理的目的和评价标准◆目的◎分离提纯得到纯的产品◆评价标准 分离提纯得到纯的产品 原料、中间体、溶剂及有价值的副产物是否最大限度的得到回收利用 后处理步骤,无论是工艺还是设备,是否足够简化 三废量是否达到最小PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/反应混合物均相非均相基本原则:有固体就过滤、有分层就分液2.后处理的常规方法PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.1不同溶剂的后处理2.1.1与水不混溶的溶剂的处理常用该类试剂有:甲苯,乙醚,乙酸乙酯,二氯甲烷等处理方法:直接旋干纯化或加水洗涤分液PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.1不同溶剂的后处理2.1.2与水混溶的溶剂的处理常用该类试剂有:乙酸,低级醇类,丙酮,乙腈,四氢呋喃(低沸)1,4-二氧六环,DMF/DMSO,吡啶,NMP等。(高沸)处理方法:旋干萃取,稀释洗涤或加水析出PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.1不同溶剂的后处理冷却,缓慢加水,析出固体过滤洗涤得到纯品过滤,旋蒸剩少量二氧六环加水析出固体,洗涤得到纯品PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.2不同底物的后处理2.2.1柔性结构化合物后处理柔性结构:指键能够自由旋转。常见的柔性结构基团有脂肪族基团如Boc/t-Bu/n-Bu等,含硅基基团,如TBS/TMS/SEM等处理处理方法:选择合适的溶剂萃取,纯化。Note:TLC板信息对后处理萃取溶剂的选择很重要PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.2不同底物的后处理2.2.2刚性结构化合物后处理刚性结构:指键不能自由旋转,原子处于同一平面。所含刚性结构的基团越多,化合物溶解度就越差。这类化合物多数为环结构或者电子容易离域大π键结构。如:并环结构大π键离域酰胺大π键离域处理方法:合适的溶剂洗涤,或者引人柔性保护基团纯化。再去保护。PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.2不同底物的后处理PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.2不同底物的后处理PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.2不同底物的后处理常用特殊试剂:LiAIH4(LAH,DIBAL-H,格式试剂等)处理前考虑的问题: 产物的稳定性以及后处理的难易程度; 所用特殊试剂的量; 淬灭过程会是否大量放热; 这类试剂参与的反应一般反应较快,检测是否及时;反应时间过长,会不会反应变杂;Note:在后处理前,推荐取一点反应液留作样品,以供后处理好的反应液对照比较。PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/LiAIH4/DIBAL-H的淬灭及后处理处理难点:反应淬灭后,产生大量不溶于水的粘性铝化合物常用淬灭剂:十水硫酸钠,乙酸乙酯/乙醇、水PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/LiAIH4/DIBAL-H的淬灭及后处理标准操作LAHLithiumAluminumHydride(xg):1.用适量乙醚稀释后冷却到0℃;2.慢慢加入xmL水;3.加入xmL15%氢氧化钠水溶液;4.再加入3xmL水;5.升温到室温搅拌15分钟;6.加入一些无水MgSO4;7.搅拌15分钟后过滤除盐。DIBAL-HDiisobutylAluminumHydride(xmmol):1.用适量乙醚稀释后冷却到0℃;2.慢慢加入0.04xmL水;3.加入0.04xmL15%氢氧化钠水溶液;4.加入0.1xmL水;5.升温到室温搅拌15分钟;6.加入一些无水MgSO4;7.搅拌15分钟后过滤除盐。PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/2.3特殊试剂的淬灭及处理GrignardReagent淬灭常用sat.NH4Cl或者冰水淬灭Note:注意淬灭时的加料顺序将反应液倒入冰水中将冰水滴加到反应液中80%-10%-95%PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/其他特殊试剂的淬灭及处理 种类 处理方法* BoronCompounds 加入MeOH,生成了(MeO)3B,旋蒸除去;BH3,在0℃用水或甲醇淬灭 PCC/PDC 通过硅藻土、硅酸镁载体等过滤除去 JonesResgent 加入异丙醇直至反应体系验收从橙色或红色变成绿色 CopperSalts 用饱和NH4Cl水溶液来淬灭反应,再在室温下搅拌一段时间至溶液呈深蓝色,分掉水相 R3Sn-XByproducts 可以通过KF与硅藻土的混合物过滤,也可以通过硅胶短柱,以反应溶剂(加~2-5%的Et3N)为洗脱剂来除去 MetalSalts 许多过滤态金属可以与硫化物生成沉淀除去。通常可以用Na2S水溶液来洗涤PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/3易燃易爆或剧毒品的后处理《常见危险废物的销毁方法》 种类 处理方法* 酰氯、三氯氧磷、氯化亚砜 在搅拌下,加到大量水中,再用碱中和 硫酸二甲酯 在搅拌下,滴加到稀NaOH或氨水中,中和 有机锂化物 溶于THF中,慢慢加入过量一倍mol的EtOH,再加水稀释,最后加稀HCL至溶液变清 氰化物 调PH>9,加入保护NaCLO溶液(1mol的约需0.4L)过夜,用亚硝酸盐试纸正式NaCLO已过量 叠氮物 调PH>9,按1:50以上的浓度配成稀的水溶液,搅拌下慢慢加入饱和NaCLO溶液(1g约需10ml)淬灭 过氧化物 在酸性水溶液中,用Fe2+、亚硫酸盐或二硫化物还原至淀粉KI试纸呈阴性,中和 碱金属氢化物、钠屑 悬浮在干燥四氢呋喃中,搅拌下慢慢加入乙醇或异丙醇至不再放出氢气、澄清为止PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/易燃易爆或剧毒品的后处理催化氢化常用的催化剂(RaneyNi,Pd/C,Pd(OH)2等)危险性:干燥时易燃,和空气或有机物的气体摩擦也容易燃烧RaneyNi>Pd/C>Pd(OH)2后处理要点:◆从高压釜抽取反应液时必须有两人在场 在快抽干时,提前解除真空,或立即加入相应的溶剂冲洗内壁,把遗留催化剂全部抽走; 抽滤时也不能完全抽干,快抽干时,接着加反应液或空白溶剂 事先准备一块湿布或一杯水,起火星时用湿布捂或用水灭 用过的催化剂或沾有这些催化剂的滤纸、塞内塑料垫等绝不能丢入垃圾桶中,应密封在容器中,用水或邮寄溶剂盖住。PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/4后处理常见文件的解决技巧4.1在萃取时常常出现不分层和乳化的现象 长时间静置; 加入适当的物质,使其密度差增大,对于水相,通常加入无机盐 因表面活性剂存在而形成的乳化,改变溶液的PH往往能使其分层; 因碱性而产生乳化,可加入少量酸破坏; 因少量悬浮固体引起的乳化,可将乳浊液缓慢过滤,过滤时在漏斗里铺上一层吸附剂(硅酸镁、氧化铝、硅胶),则效果更好;⑥对于顽固的乳化,还可用离心分离,也可加热,或向有机溶剂中加入极性溶剂(如醇类或丙酮)以改变两相的表面张力。PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/4后处理常见解决技巧4.2关于有机反应中油状物的处理固体产物呈油状物原因: 产物很不纯,有很多杂质; 产物中含有溶剂,特别是包含了高沸点的溶剂; 产物熔点较低,有含有一些溶剂,熔程变大而不易结晶。 析晶过快解决方法: 用低沸点的溶剂尽量把溶剂带干; 高真空油泵抽气除去高沸点溶剂,含水的话,也可以考虑冻干; 加入良性溶剂(沸点较低)溶解后,再加入不良溶剂(要筛选),然后不加热缓慢旋走部分良性溶剂,若还不析出,可冷却或用超声波超一下;d)用溶剂重结晶。e)柱层析纯化得精种*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/4后处理常见文件的解决技巧4.3抽滤时滤饼很粘稠怎么办? 打碳层,或者硅藻土层; 加助滤剂(硅胶、氧化铝、无水硫酸钠等); 沉降法,放置一段时间,先滤上层清夜; 勤换滤纸; 换用滤布; 离心法。 用棉花过滤4.4如何除去过量的(Boc)2O? 若产物极性较大,可用Hexane或乙醇萃取除去; 加入少量N,N-二甲基丙二胺(或N,N-二甲基乙二胺),待TLC检测过量的(Boc)2O(一般10:1,Rf~0.6左右,以碘显色)消失后,以1M稀盐酸洗涤(如果担心Boc的安全就用10%的柠檬酸洗)。*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理5.1含铝化合物反应的后处理 Friedel–Craftsreaction产物耐酸,将反应液缓慢倾入含盐酸的冰水中,然后后处理。产物对酸敏感,将反应液缓慢倾入冰水中,加入有机溶剂,然后过滤除去不容物。过滤时铺硅藻土。 氢锂铝参与的反应先用水淬灭,淬灭时注意氮气保护,然后以上面方法进行后处理。5.2双键顺式氧化为邻二醇1.高锰酸钾顺式氧化为邻二醇2.催化量四氧化饿和双氧水或者催化量的饿酸钾加双氧水顺式氧化为邻二醇跟NMO配合用,OsO4只需要5-10mol,反应在THF:tBuOH:H2O=4:1:1混合溶剂里进行,室温,过夜反应。后处理用Na2SO3溶液洗涤。水相用EtOAc萃取若干次。*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理5.3氧化反应的后处理1.高锰酸钾参与的氧化反应1)反应的过程中产生大量的二氧化锰,是整个体系变的难搅拌,后处理时难过滤,一般在反应中加入一定量的硅藻土。2)用还原性的无机盐淬灭反应,一般亚硫酸钠溶液,亚硫酸氢钠溶液和硫代硫酸钠溶液。2.醇氧化成相应的酮或者醛氧化剂:PCC,PDC,戴斯马丁氧化剂,Swern氧化,NaClO溶液+TEMPO,TCCA+TEMPO1)用PCC,PDC等重金属氧化剂时,反应液中加入硅藻土,反应完全后过滤,柱层析纯化得目标产物2)用NaClO溶液+TEMPO,TCCA+TEMPO作氧化剂时,注意控制加料速。反应完全用还原性试剂淬灭反应。*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理淬灭试剂的选择用NaClO溶液+TEMPO氧化时用硫代硫酸钠溶液淬灭用TCCA+TEMPO作氧化剂时,可用碳酸氢钠溶液或者硫代硫酸钠溶液淬灭1)LHA和R1MgX,R1Li的量小于1eq,且缓慢加入。反应时间一般小于1h.2)反应完全后立即用水,控温下淬灭反应。3Weinreb酰胺的还原*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理5.4硝化反应的后处理反应完全后,将反应液缓慢倾入大量的碎冰中,此时有黄色固体析出,过滤,水洗涤得目标产物。5.5Wittig反应 合成叶立德时,加入硅藻土,否则反应液搅拌困难2)反应完全后减压浓缩,柱层析得目标产物或者用石油醚(正己烷)提取产物*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理5.4卤化反应的后处理1.NBS或者NIS的卤化1)反应完全后,将反应液倾入水中,若有固体析出,则过滤,水洗涤得产品。2)若没有析出固体,则用有机溶剂萃取,然后用硫代硫酸钠洗涤有机相,饱和食盐水洗涤两次。注意:使用NBS或者NIS时要避光。2.溴素溴代 反应完全后直接过滤,醋酸洗涤,水洗涤至中性。 酰氯法合成a-溴代酸是:反应完全后减压除去过量的溴素和溶剂,然后用乙酸乙酯溶解残余物,缓慢加入水淬灭,饱和食盐水洗涤。*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理5.5酰胺脱水成氰基1.酰胺的脱水反应可在TFFA-TEA,TFFA,POCl3,SO2Cl2,P2O5,PCl3,(COCl)2-NEt3-DMSO,CH3SO2Cl,TiCl4,Bugess试剂等脱水剂存在下进行脱水反应生成腈,此为实验室合成腈的方法之一。具体例子见附件2.POCl3(Vilsmeier试剂)合成酰胺后处理1)控制温度,缓慢向反应液中滴加水淬灭反应;2)用碳酸钠溶液调节pH至7-8,然后有机相机萃取,水洗的有机相的DMF。*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理3.三聚氯氰合成氰基化合物后处理1)控制温度,缓慢向反应液中滴加水淬灭反应;2)用碳酸钠溶液调节pH至7-8,然后有机相机萃取;3)过滤除去大量的不溶物,然后有机溶剂萃取,有机相用碳酸氢钠溶液洗涤杂质,饱和食盐水洗涤有机相中的DMF。注意:加料过程佩戴防毒面具。1)叠氮化钠遇金属和猛烈撞击易发生爆炸2)含叠氮化钠的废液应该处理:用次氯酸钠水溶液处理终点用碘化钾淀粉试纸判断。5.6NaN3合成氨*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理1.酸性试剂1)常见酸性脱甲基试剂:浓HI酸,大大过量的48%的HBr酸溶液或者37%的HCl溶液在Hac或者醋酸酐中回流。2)反应完全后加入大量的水,有机溶剂萃取,然后进一步纯化。2.路易斯酸1)常见的脱甲基路易斯酸,AlCl32)反应完全后,将反应液倾入水中,加入6M的盐酸酸化,有机溶剂萃取,进一步纯化。3.其他的脱甲基试剂5.7甲基醚的脱甲基反应*PPT模板下载:www.1ppt.com/moban/行业PPT模板:www.1ppt.com/hangye/节日PPT模板:www.1ppt.com/jieri/PPT素材下载:www.1ppt.com/sucai/PPT背景图片:www.1ppt.com/beijing/PPT图表下载:www.1ppt.com/tubiao/优秀PPT下载:www.1ppt.com/xiazai/PPT教程:www.1ppt.com/powerpoint/Word教程:www.1ppt.com/word/Excel教程:www.1ppt.com/excel/资料下载:www.1ppt.com/ziliao/PPT课件下载:www.1ppt.com/kejian/范文下载:www.1ppt.com/fanwen/试卷下载:www.1ppt.com/shiti/教案下载:www.1ppt.com/jiaoan/5常见反应的后处理1.反应底物保持中性2.(Boc)2O的量不大于1eq,且反应完全后,立即处理。3.淬灭反应用10%的柠檬酸溶液,有机相洗至中性。5.8吲哚环Boc保护************
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