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    • 4. 发明授权
    • Process for preparing alkyladamantyl esters and compositions
    • 烷基金刚烷酯和组合物的制备方法
    • US07026504B2
    • 2006-04-11
    • US10470126
    • 2001-01-26
    • Masao YamaguchiHiromasa YamamotoHideki KikuchiYoshihiro Hirota
    • Masao YamaguchiHiromasa YamamotoHideki KikuchiYoshihiro Hirota
    • C07C69/52
    • C07C67/60C07C2603/74G03F7/0397C07C69/54C07C69/013
    • There is provided a method for obtaining a high-purity alkyladamantyl ester from an alkyladamantyl ester composition containing a large quantity of alkyladamantyl halide obtained by, for example, alkylating raw material 2-adamantanone obtained through oxidation of adamantane by use of an organic metal reagent and then causing an acid halide to react with the resulting product, efficiently by a simple process. To an alkyladamantyl ester composition containing an alkyladamantyl halide such as 2-chloro-2-methyladamantane in an amount of larger than 0.5 parts by weight based on 100 parts by weight of alkyladamantyl ester such as 2-methyl-2-adamantyl methacrylate, a mixed solution of, for example, methanol and a sodium hydroxide aqueous solution is added. By bringing the alkali compound into contact with the alkyladamantyl halide in a homogeneous system so as to convert the halide into a compound which produces no acid when heated, the amount of the alkyladamantyl halide in the composition is reduced to 0.5 parts by weight or less based on 100 parts by weight of the alkyladamantyl ester, after which distillation is carried out.
    • 提供了一种从含有大量烷基金刚烷基卤化物的烷基金刚烷基酯组合物中获得高纯度烷基金刚烷基酯的方法,所述烷基金刚烷基酯通过使用有机金属试剂将金刚烷氧化而得到的原料2-金刚烷烷化, 然后通过简单的方法使酰基卤与所得产物反应。 对于基于100重量份的烷基金刚烷基酯如甲基丙烯酸2-甲基-2-金刚烷基酯,含有烷基金刚烷基卤化物如2-氯-2-甲基金刚烷的量大于0.5重量份的烷基金刚烷基酯组合物,混合 加入例如甲醇和氢氧化钠水溶液的溶液。 通过使碱性化合物与均匀体系中的烷基金刚烷基卤化物接触,以便将卤化物转化为加热时不产生酸的化合物,组合物中烷基金刚烷基卤化物的量降低至基于0.5重量份或更少 在100重量份的烷基金刚烷基酯上进行蒸馏。
    • 7. 发明授权
    • Production method of high purity organic compound
    • 高纯度有机化合物的生产方法
    • US06852885B2
    • 2005-02-08
    • US10296319
    • 2001-01-26
    • Hiromasa YamamotoMasao YamaguchiHideki Kikuchi
    • Hiromasa YamamotoMasao YamaguchiHideki Kikuchi
    • C07C67/54C07D275/02C07D67/52C07D67/54
    • C07C67/54C07C2603/74C07C69/54
    • There is provided a method for obtaining a target organic compound such as an alkyladamantyl ester efficiently by purifying a crude organic compound which contains, as impurities, sublimable materials which start to sublime at temperatures lower than a boiling point of the target organic compound by use of such a simple method as distillation during its production process, without being adversely affected by adherence of the sublimable materials.The distillation is carried out in the presence of a compound having a boiling point which is lower than a boiling point of the target organic compound, e.g., a carbonyl-group-containing compound. For example, 2-methyl-2-adamantyl methacrylate (boiling point: 92° C./0.3 mmHg) containing sublimable impurities such as adamantane (sublimation starting temperature: room temperature or lower) is distilled in the presence of 1,3-dimethyl-2-imidazolidinone (boiling point: 225° C.).
    • 提供了一种通过纯化粗制有机化合物来有效地获得目标有机化合物如烷基金刚烷基酯的方法,所述粗制有机化合物含有作为杂质的可升华材料,其在低于目标有机化合物的沸点的温度下开始升华, 这种简单的方法是在其生产过程中的蒸馏,而不受升华材料的粘附的不利影响。蒸馏在沸点低于目标有机化合物的沸点的化合物的存在下进行, 例如含羰基化合物。 例如,将含有金刚烷(升华开始温度:室温以下)的升华性杂质的甲基丙烯酸2-甲基-2-金刚烷酯(沸点:92℃/ 0.3mmHg)在1,3-二甲基 -2-咪唑啉酮(沸点:225℃)。