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    • 63. 发明申请
    • METHOD OF CRYSTALLIZATION AND PURIFICATION FOR OBTAINING STABE 'beta' CRYSTAL OF TETRAKIS[3-(3,5-DI-TERTIARY-BUTYL-4-HYDROXYPHENYL)PROPIONYLOXYMETHYL]METHANE ON AN INDUSTRIAL SCALE
    • 用于获得TETRAKIS的稳定化和纯化方法[3-(3,5-二叔丁基-4-羟基苯基)丙炔基]甲基]工业规模甲烷
    • WO1989009202A1
    • 1989-10-05
    • PCT/JP1989000333
    • 1989-03-29
    • YOSHITOMI PHARMACEUTICAL INDUSTRIES, LTD.NARITA, TadatsuguMARUNO, Makoto
    • YOSHITOMI PHARMACEUTICAL INDUSTRIES, LTD.
    • C07C69/732
    • C07C67/48C07C69/732
    • An industrial method for crystallizing and purifying tetrakis[3-(3,5-di-tertiary-butyl-4-hydroxyphenyl)propionyloxymethyl]methane which comprises stabilizing the beta crystal structure produced by dissolving in a water-soluble solvent under reflux a reaction mixture containing tetrakis [3-(3,5-di-tertiary-butyl-4-hydroxyphenyl)propionyloxymethyl]methane obtained by transesterification between pentaerythritol and a lower alkyl ester of 3-(3,5-di-tertiary-butyl-4-hydroxyphenyl)propionic acid crystallizing the obtained solution by pouring it into a cooled solvent composed of a water-soluble solvent in an amount 0.2 - 1.5 times by weight of the reaction mixture and water in an amount 0.06 - 0.09 time by weight of the water-soluble solvent. This method will not cause operational inconveniences such as scaling and incapability of agitation resulting from particle size reduction. It is also possible to manufacture, with stability and ease, the aforementioned compounds in the form of beta crystal which is white in color, excellent in hue and practically satisfactory in purity, on an industrial scale.
    • 一种用于结晶和纯化四[3-(3,5-二叔丁基-4-羟基苯基)丙酰氧基甲基]甲烷的工业方法,其包括将通过在回流下溶解在水溶性溶剂中而产生的β晶体结构稳定反应混合物 通过季戊四醇与3-(3,5-二叔丁基-4-羟基苯基)的低级烷基酯的酯交换得到的含有四[3-(3,5-二叔丁基-4-羟基苯基)丙酰氧基甲基]甲烷的四[ )丙酸将所得溶液倒入由反应混合物重量的0.2〜1.5倍的水溶性溶剂组成的冷却溶剂中,水的重量计为0.06〜0.09倍 溶剂。 该方法不会引起诸如由于粒径减小引起的搅动和搅拌不能引起的操作上的不便。 也可以以稳定和容易的方式制造上述化合物,其为白色,白色,色纯度优异,纯度实际满意的β晶型。