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C.tert-Butylaminehydrochloride.Ina2-l.flaskfittedwithanefficientbulb-typerefluxconden...
C. tert-Butylamine hydrochloride. In a 2-l. flask fitted with an efficient bulb-type reflux condenser are placed 203 g. (1 mole) of tert-butylphthalimide, 1 l. of 95% ethanol, and 59 g. (1 mole) of 85% hydrazine hydrate. The solution is refluxed for 2 hours and cooled, and concentrated hydrochloric acid (about 100 ml.) is added until the solution is strongly acid to Congo red paper, though a large excess of acid is avoided. The voluminous precipitate of phthalhydrazide is collected on a 15-cm. Büchner funnel with the aid of suction and washed with four 100-ml. portions of 95% ethanol. The combined filtrate and washings are concentrated under reduced pressure to a volume of 200 ml. About 1 l. of water is added, any insoluble material is removed by filtration, and the filtrate is concentrated to about 300–350 ml. If any additional insoluble material separates it is removed by filtration, and the solvent is completely removed by evaporation under reduced pressure. This crude amine hydrochloride may be converted to the free amine as described below, or it may be purified by solution in 500 ml. of absolute ethanol, the solution being filtered and 500 ml. of dry ether being added to the filtrate. The crude amine hydrochloride is collected on a filter; the solvent is removed by suction, and the residue is dissolved in hot absolute ethanol using 5 ml. per gram of material; absolute ether (50% of the volume of ethanol) is added, and the solution is cooled in a refrigerator for several hours. All the tert-butylamine hydrochloride is collected on a Büchner funnel and dried in a vacuum desiccator. It weighs 79–97 g. (72–88%) and melts with sublimation at 270–290°.
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花了我半小时,下次挑重点问,不要一大段都贴上来。
叔丁胺盐酸盐的合成。
在装有球型回流冷凝器的2升瓶中加入203克(1摩尔)叔丁基邻苯二甲酰亚胺,一升95%的乙醇和59克(1摩尔)的85%水合肼。溶液加热至回流2小时,冷却,加入盐酸(约100毫升。)调节溶液ph至刚果红试纸显强酸性,但酸不要过量。将反应产生的大量沉淀物邻苯二甲酰肼收集到直径15厘米的布氏漏斗中,并用4x100ml 95%乙醇冲洗。合并滤液和洗液,减压浓缩至约200毫升。加入1升水,过滤去除掉任何不溶性物质,再将滤液浓缩至约300-350毫升。如果再有不溶性物质出现仍然用过滤方法将其除去,然后减压蒸除所有溶剂。粗品胺盐酸盐按如下方法精制:将粗品溶解于500毫升无水乙醇,过滤除去不容物,滤液中加入500ml干乙醚。
具体如下:粗胺盐酸盐用无水乙醇溶解,每克粗品约用无水乙醇5毫升,加入绝对乙醚(乙醇量的50%),将以上溶液在冰箱冷却析晶几个小时。将所有的纯品叔丁胺盐酸盐用布氏漏斗过滤收集,并在真空干燥器中干燥。重量约为79-97克(72-88%),熔点270-290 并升华。
叔丁胺盐酸盐的合成。
在装有球型回流冷凝器的2升瓶中加入203克(1摩尔)叔丁基邻苯二甲酰亚胺,一升95%的乙醇和59克(1摩尔)的85%水合肼。溶液加热至回流2小时,冷却,加入盐酸(约100毫升。)调节溶液ph至刚果红试纸显强酸性,但酸不要过量。将反应产生的大量沉淀物邻苯二甲酰肼收集到直径15厘米的布氏漏斗中,并用4x100ml 95%乙醇冲洗。合并滤液和洗液,减压浓缩至约200毫升。加入1升水,过滤去除掉任何不溶性物质,再将滤液浓缩至约300-350毫升。如果再有不溶性物质出现仍然用过滤方法将其除去,然后减压蒸除所有溶剂。粗品胺盐酸盐按如下方法精制:将粗品溶解于500毫升无水乙醇,过滤除去不容物,滤液中加入500ml干乙醚。
具体如下:粗胺盐酸盐用无水乙醇溶解,每克粗品约用无水乙醇5毫升,加入绝对乙醚(乙醇量的50%),将以上溶液在冰箱冷却析晶几个小时。将所有的纯品叔丁胺盐酸盐用布氏漏斗过滤收集,并在真空干燥器中干燥。重量约为79-97克(72-88%),熔点270-290 并升华。
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