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href=\"\u002Fen\u002Fcas\u002F24424-99-5_401983.html#duXinDiv\">二碳酸二叔丁酯毒性英文版\u003C\u002Fa>\u003C\u002Fp>\n\n\u003C\u002Ftd>","\u003Cp>1.叔丁醇钾溶于无水四氢呋喃，在-5～-20℃通入干燥的二氧化碳，生成浆状物，继续保持低温，滴加光气苯溶液，制得三碳酸二叔丁酯。将其溶于四氯化碳，加适量1,4-二氮杂二环[2,2,2]辛烷，在25℃搅拌使二氧化碳释放完全，转化为二碳酸二叔丁酯。\u003C\u002Fp>\u003Cp>2.注意！使用剧毒性的光气，应在通风厨内小心操作。凡粘有光气溶掖的玻璃器皿，均应清洗后方可拿出通风橱。\u003Cbr \u002F>(1)制三碳酸二叔丁酯\u003Cbr \u002F>将装有机械搅拌器，200毫升恒压滴压漏斗，氯化钙干燥管，伸近瓶底的内径不小于6毫米的1升三颈烧瓶烘干。事先校准并标出滴液漏斗盛装85毫升和105毫升液体的水平面。通入干燥氮气，烧瓶中加入44.8克(0.40摩尔)不含醇的叔丁醇钾和550毫升无水四氢吠喃，搅拌5-10分钟使成溶液。将反应瓶浸入冰盐浴以保持-5一-20℃，在剧烈搅拌下，通入干燥二氧化碳，大约30分钟，生成稠密的浆状物。与此同时，将86毫升无水苯加入滴液漏斗中，并鼓入光气泡，直到光气在苯中的溶液体积达105毫升为止，相当于含有24克(0.24摩尔)的光气。当二氧化碳的加成反应完成后，在剧烈搅拌下将光气溶液滴加到冷却的反应物中，约需1小时，冷浴温度保持在-5~-10℃，反应混合物粘度变小，仍为白色乳状物。当光气的加成反应完成后，继续搅拌，45分钟，同时通入无水氮乙毛以吹出大部分的过量光气。卸除烧瓶上的仪器，塞上二颈，在减压下用旋转蒸发器将约650毫升溶剂浓缩至100毫升，烧瓶仍用冰盐浴冷却以保持一5一0℃。由于反应混合物中残余少量光气，应将抽气泵或真空泵废气排入通风橱，收集在冷阱中的物料也在通风橱内抽空，含有很细分散的氯化钾的残余物用大口径砂芯漏斗吸滤，漏斗在用前经50毫升冰冷的戊烷进行预冷。过滤时，用一个大口径漏斗将过滤漏斗反盖着，并通入氮气使物料隔除潮湿空气，用J}}毫升冰冷的戊烷将烧瓶中残余物洗入过滤漏斗中，然后用2*100毫升冰冷的戊烷洗涤滤渣。滤液与戊烷洗涤液合并，在0℃减压下，用旋转蒸发器浓缩至于，得白色固体，重33.7克,将粗品溶于1250毫升戊烷，冷至-15℃ ,拆出白色晶体。母液经旋转蒸发器浓缩后还可得到两批晶体，总计得到三碳酸二叔丁酯纯品31.2-32.8(59~62%)，为白色晶体，熔点 62~63℃(分解)。\u003Cbr \u002F>(2)制二碳酸二叔丁酚\u003Cbr \u002F>在放有电磁搅拌棒的烧杯中，加入20.0克（0 .076摩尔)三碳酸二叔丁醋溶于了i}毫升四氯化碳的溶液和0.10克(0.0009摩尔)新升华的1.4一二氮杂二环〔2·2·2〕辛烷，立即迅速地释放出二氧化碳。在25℃搅拌45分钟使二氧化碳释放完全，然后加入足以使水层为弱酸性的含有适量柠檬酸的35毫升水溶液。分出有机层，用无水硫酸镁干燥，在25℃用旋转蒸发器浓缩，残余液经减压蒸馏，得到二碳酸二叔丁酚无色液体产13.3---15.1克(80~91%)用三乙胺作催化剂也得到类似结果。但三乙胺不如1,4-二氮杂二环辛烷有效，因为三乙胺与溶剂可能反应，且与产物的分离较困难。\u003C\u002Fp>\u003Cp>3.在1,4-二氮杂二环[2.2.2]辛烷的催化下，将碳酰氯与碳酸叔丁酯直接反应而制备。\u003C\u002Fp>","2026-08-21T07:51:12.859463Z",false,[397,403,409,415,421,427],{"slug":398,"cid":399,"name":400,"nameZh":401,"cas":402},"785894228747096064","J-1501481-0","3-[2-(Trifluoromethyl)phenyl]propanoic acid","3-[2-(三氟甲基)苯基]丙酸","94022-99-8",{"slug":404,"cid":405,"name":406,"nameZh":407,"cas":408},"785903777449250816","J-873302-3","Calcium bis(2-fluoroprop-2-enoate)","双(2-氟丙-2-烯酸)钙","1208912-83-7",{"slug":410,"cid":411,"name":412,"nameZh":413,"cas":414},"785883127103885312","J-7142-4","2,2,3,3,3-Pentafluoropropyl methacrylate","甲基丙烯酸2,2,3,3,3-五氟丙酯","45115-53-5",{"slug":416,"cid":417,"name":418,"nameZh":419,"cas":420},"854303161911873536","J-1135619-6","N-cyclohexylcyclohexanamine,hydrochloride","二环己胺盐酸盐","4693-92-9",{"slug":422,"cid":423,"name":424,"nameZh":425,"cas":426},"785875657052655616","J-1133573-3","2-(3,4-dimethoxyphenyl)ethanamine hydrochloride","2-(3,4-二甲氧基苯基)乙胺盐酸盐","635-85-8",{"slug":428,"cid":429,"name":430,"nameZh":431,"cas":432},"785881853994209280","J-1133334-8","diphenylmethanimine hydrochloride","二苯甲酮亚胺盐酸盐","5319-67-5",1792607957846,"zh-CN",[]]