首页> 外国专利> PREPARATION OF ASCORBIC ACID-2-PHOSPHATE, AND PREPARATION OF POTASSIUM MAGNESIUM-L-ASCORBATE-2- PHOSPHATE, K1+-0.3 MG1+-0.15-L-ASCORBATE-2-PHOSPHATE AND 5,6-ISOPROPYLIDENE-ASCORBIC ACID

PREPARATION OF ASCORBIC ACID-2-PHOSPHATE, AND PREPARATION OF POTASSIUM MAGNESIUM-L-ASCORBATE-2- PHOSPHATE, K1+-0.3 MG1+-0.15-L-ASCORBATE-2-PHOSPHATE AND 5,6-ISOPROPYLIDENE-ASCORBIC ACID

机译:抗坏血酸-2-磷酸酯的制备,钾镁-L-抗坏血酸-2-磷酸酯,K1 + -0.3 MG1 + -0.15-L-抗坏血酸-2-磷酸酯和5,6-异丙烯基-抗坏血酸

摘要

Process for the preparation of ascorbic acid 2-phosphate by reacting ascorbic acid or ascorbic acid derivatives with POCl3 in the presence of a tertiary amine in an appropriate aqueous solvent at temperatures of -10 to 25 DEG C, while maintaining a pH of about 8 to 13.5 with KOH throughout the whole phosphorylation reaction and subsequently isolating of the ascorbic acid 2-phosphate, characterised in that the reaction mixture produced on phosphorylation is treated with the aqueous solution of a magnesium compound without previous ion exchange treatment until the formation of crystalline KMgPO4 has terminated, the crystallised KMgPO4 is separated off, the filtrate so obtained is concentrated at a pH of 6 to 11 and/or treated with 0.1 to 5 times the amount, relative to the concentrated filtrate, of a primary lower alkanol or acetone, and cooled with stirring until the KCl has stopped crystallising out, and the ascorbic acid phosphate is isolated in a known way from the reaction solution, obtained after separating off KCl, which is largely free of inorganic salts. It is especially advantageous to isolate the ascorbic acid 2-phosphate in the form of the new potassium magnesium ascorbate 2-phosphate, for which patent protection is also applied for. The process is especially advantageous if 5,6-isopropylidene- ascorbic acid is used as the ascorbic acid derivative, this being obtained by reacting ascorbic acid with acetone in the presence of oleum. The process is of particular importance for the preparation of L-ascorbic acid 2-phosphate.
机译:通过使抗坏血酸或抗坏血酸衍生物与POCl3在叔胺存在下,在适当的水性溶剂中,在-10至25℃的温度下,同时保持pH值为约8至25的条件下制备抗坏血酸2-磷酸的方法13.5在整个磷酸化反应中用KOH进行分离,然后分离出抗坏血酸2-磷酸酯,其特征在于,将磷酸化反应中生成的反应混合物用镁化合物的水溶液处理,而无需事先进行离子交换处理,直到形成结晶的KMgPO4为止。终止,分离出结晶的KMgPO 4,将所得滤液在pH 6至11下浓缩和/或用相对于浓缩滤液0.1至5倍量的低级伯烷醇或丙酮处理,并冷却在搅拌下直至KCl不再结晶出来,并以已知方式从反应溶液中分离出抗坏血酸磷酸酯,分离出基本上不含无机盐的氯化钾后得到的产物。以新的抗坏血酸钾镁2-磷酸酯的形式分离抗坏血酸2-磷酸酯是特别有利的,对此也申请了专利保护。如果使用5,6-异亚丙基-抗坏血酸作为抗坏血酸衍生物,则该方法是特别有利的,这是通过在发烟硫酸存在下使抗坏血酸与丙酮反应而获得的。该方法对于制备L-抗坏血酸2-磷酸酯特别重要。

著录项

  • 公开/公告号JPH02286693A

    专利类型

  • 公开/公告日1990-11-26

    原文格式PDF

  • 申请/专利权人 BASF AG;

    申请/专利号JP19900068496

  • 申请日1990-03-20

  • 分类号C07F9/655;

  • 国家 JP

  • 入库时间 2022-08-22 06:01:20

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