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    • 1. 发明授权
    • Process for the preparation of
6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and for the
purification thereof
    • 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物的制备方法及其纯化方法
    • US4804755A
    • 1989-02-14
    • US902427
    • 1986-08-29
    • Dieter ReuschlingAdolf LinkiesWalter ReimannOtto E. SchweikertKarl E. MackWolfgang Ebertz
    • Dieter ReuschlingAdolf LinkiesWalter ReimannOtto E. SchweikertKarl E. MackWolfgang Ebertz
    • A23L27/20A23L27/30C07D291/06
    • C07D291/06
    • The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxothiazin-4-one 2,2-dioxide are prepared by cyclizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert inorganic solvent, hydrolyzing the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide obtained in the form of the SO3-adduct after the cyclization reaction, in the event that the amount of SO3 employed is more than equimolar, purifying the organic phase (which has separated out) by extraction with a small volume of water or dilute aqueous sulfuric acid, preferably only with water, and isolating, by neutralization with bases, the non-toxic salts of the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide from the organic phase thus purified.The said salts are obtained in this process in an extremely pure form; they are valuable synthetic sweetening agents. The potassium salt is known as acesulfam (K).
    • 6-甲基-3,4-二氢-1,2,3-氧代噻嗪-4-酮2,2-二氧化物的无毒盐通过将乙酰乙酰胺-N-磺酸或其盐与至少大约 在与水不混溶的惰性有机溶剂存在下等摩尔量的SO 3,如果合适的话也可以是惰性无机溶剂,水解6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮 在环化反应后以SO 3 - 加合物的形式获得的二氧化二氮,在所用SO 3的量大于等摩尔的情况下,通过用少量体积的萃取纯化有机相(其分离出来) 水或稀硫酸水溶液,优选仅用水,并通过与碱中和,分离出6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2的无毒盐, 从有机相中纯化二氧化碳。 所述盐在该方法中以非常纯的形式获得; 它们是有价值的合成甜味剂。 钾盐被称为乙酰磺胺酸(K)。
    • 6. 发明授权
    • Process for the preparation of
6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and for the
purification thereof
    • 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物的制备方法及其纯化方法
    • US4806639A
    • 1989-02-21
    • US902206
    • 1986-08-29
    • Dieter ReuschlingAdolf LinkiesWalter ReimannOtto E. SchweikertKarl E. Mack
    • Dieter ReuschlingAdolf LinkiesWalter ReimannOtto E. SchweikertKarl E. Mack
    • A23L27/20A23L27/30C07D291/06
    • C07D291/06
    • 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by cylcizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO.sub.3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert, inorganic solvent. In the event that an equimolar amount of SO.sub.3 is employed, working up is effected by adding aqueous sulfuric acid when the cyclization reaction is complete; in the event that the amount of SO.sub.3 employed is more than equimolar, the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide obtained in the form of the SO.sub.3 -adduct is hydrolyzed by adding water or ice, whereby sulfuric acid is formed from the SO.sub.3 combined in the SO.sub.3 -adduct.The inert, organic solvent is then removed from the resulting multi-phase mixture by distillation, and the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is obtained in a pure form from the remaining aqueous sulfuric acid phase by crystallization. Additionally, quite generally, crude 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is purified by recrystallization from aqueous sulfuric acid. The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2 dioxide--in particular the potassium salt--are valuable synthetic sweetening agents.
    • 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物是通过将乙酰乙酰胺-N-磺酸或其盐与至少约等摩尔量的SO 3进行环烷酸 存在不溶于水的惰性有机溶剂,并且如果合适,也是惰性的无机溶剂。 在使用等摩尔量的SO 3的情况下,当环化反应完成时,通过加入硫酸水溶液进行加工; 在使用的SO 3的量超过等摩尔的情况下,以SO 3加合物的形式获得的6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物 通过加入水或冰水解,从而在SO 3加合物中组合的SO 3形成硫酸。 然后通过蒸馏从所得多相混合物中除去惰性有机溶剂,并将6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物 通过结晶从剩余的硫酸水相中纯化形式。 另外,通常,通过从硫酸水溶液中重结晶来纯化粗制的6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物。 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮二氧化物(特别是钾盐)的无毒盐是有价值的合成甜味剂。