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    • 139. 发明授权
    • Process for the preparation of crystalline sodium paraformylphenolate
    • 制备结晶多聚甲酚钠的方法
    • US4346238A
    • 1982-08-24
    • US147678
    • 1980-05-07
    • Alain SchouteetenYani Christidis
    • Alain SchouteetenYani Christidis
    • C07C45/00C07C45/39C07C47/565C07C47/575C07C67/00C07C45/54
    • C07C47/565C07C45/39
    • Sodium paraformylphenolate crystallized with two molecules of water is manufactured by:(a) condensing glyoxylic acid with an excess of phenol in water in the presence of sodium hydroxide at a temperature comprised between 30.degree. C. and 100.degree. C.;(b) neutralizing the solution thus obtained and then freeing it from the unconverted phenol by steam distillation or extraction with a water-immiscible organic solvent and then subjecting it hot under a pressure of oxygen, to a catalytic decarboxylating oxidizing degradation in the presence of sodium hydroxide;(c) allowing the aqueous solution so-obtained, after removal of the catalyst by filtration, and then concentration hot under vacuum to 60% plus or minus 10% of its initial volume, to crystallize; and(d) draining the precipitated crystals, washing them and then drying them to constant weight under vacuum of 1 mm of mercury at 20.degree. C., to obtain sodium paraformylphenolate crystallized with 2 molecules of water or dried to constant weight under a vacuum of 1 mm of mercury at 100.degree. C. to obtain it in anhydrous form. The product is useful for preparing parahydroxy benzaldehyde quantitatively and without other purification reactions.
    • 用两分子水结晶的多聚甲硫醇钠是通过以下方法制造的:(a)在氢氧化钠存在下,在30℃至100℃的温度下,使乙醛酸与过量的苯酚在水中冷凝; (b)中和所得溶液,然后通过水蒸气蒸馏或与水不混溶的有机溶剂萃取,然后将其从未转化的苯酚中释出,然后在氧气压力下热处理,在钠存在下进行催化脱羧氧化降解 氢氧化物; (c)通过过滤除去催化剂后,使真空度为60%±10%,使其结晶,得到如此得到的水溶液。 和(d)排出沉淀的晶体,洗涤,然后在20℃下在1mm汞柱的真空下将其干燥至恒重,得到用2分子水结晶的多聚甲酰基苯酚钠,或在真空下干燥至恒重 在100℃下加入1毫米汞柱,以无水形式得到。 该产品可用于定量和无其他纯化反应制备对羟基苯甲醛。