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    • 4. 发明授权
    • Process for the preparation of 3-hydroxybenzoic acid
    • 3-羟基苯甲酸的制备方法
    • US4393234A
    • 1983-07-12
    • US378922
    • 1982-05-17
    • Heinz U. BlankEike GabelErnst GoldschmittWerner Mentzel
    • Heinz U. BlankEike GabelErnst GoldschmittWerner Mentzel
    • C07C51/367C07C65/05C07C65/04
    • C07C309/00C07C51/367
    • 3-Hydroxybenzoic acid is obtained by reaction with an alkali metal hydroxide at a temperature of 220.degree. to 450.degree. C. and under a pressure of 1 to 120 bars, from a technical 3-sulphobenzoic acid mixture which contains sulphuric acid and/or sulphur trioxide and which contains at least 75% by weight of 3-sulphobenzoic acid, relative to the total organic constituents present, and not more than 35% by weight of sulphuric acid and/or SO.sub.3, relative to the total mass. For this purpose, this technical 3-sulphobenzoic acid mixture, if desired after dilution with an equal volume of water, is mixed with sufficient 50 to 100% strength by weight alkali metal hydroxide wherein the remaining 50 to 0% by weight consists essentially of water, for 2.5 to 8 mols of alkali metal hydroxide to be present per mol of 3-sulphobenzoic acid, after neutralization of the sulphuric acid and all the sulpho and carboxyl groups. In general, 10 to 45% by weight of water are present in the batch. The reaction mixture is acidified with a mineral acid to a pH value of less than 4, if appropriate after dilution with water, and the 3-hydroxybenzoic acid is isolated at temperatures within the range from -5.degree. C. to +40.degree. C.
    • 通过在含有硫酸和/或硫的工业3-磺基苯甲酸混合物的温度在220-450℃和1至120巴的压力下与碱金属氢氧化物反应获得3-羟基苯甲酸 三氧化硫,相对于存在的总有机成分含有至少75重量%的3-磺基苯甲酸,相对于总质量不超过35重量%的硫酸和/或SO 3。 为此目的,如果需要,在等体积水稀释后,将该技术性3-磺基苯甲酸混合物与足量的50至100%重量的碱金属氢氧化物混合,其中剩余的50至0重量%基本上由水 对于每摩尔3-磺基苯甲酸存在的2.5至8摩尔碱金属氢氧化物,中和硫酸和所有磺基和羧基后。 通常,批料中存在10至45重量%的水。 如果在用水稀释后,将反应混合物用无机酸酸化至pH值小于4,并且在-5℃至+ 40℃的温度下分离出3-羟基苯甲酸。
    • 6. 发明授权
    • Preparation of .alpha.-ketocarboxylic acid N-tert.-butylamides
    • α-酮羧酸N-叔丁基酰胺的制备
    • US4345100A
    • 1982-08-17
    • US222222
    • 1981-01-02
    • Gerhard BonseHeinz U. Blank
    • Gerhard BonseHeinz U. Blank
    • C07C231/06C07C67/00C07C231/00C07C235/72C07D253/075C07C102/08
    • C07D253/075
    • A process for the preparation of an .alpha.-ketocarboxylic acid N-tert.-butylamide of the formulaR--CO--CO--NH--C(CH.sub.3).sub.3in whichR is an aliphatic radical with up to 8 carbon atoms, a cycloalkyl radical with 3 to 6 carbon atoms, a phenyl or naphthyl radical or a heterocyclic radical,comprising reacting an acyl cyanide of the formulaR--CO--CNwith tert.-butyl methyl ether of the formula(CH.sub.3).sub.3 C--O--CH.sub.3at a temperature between about 0.degree. and 80.degree. C. in the presence of an acid which is capable of activating the ether of formula (III) under the reaction conditions to give a tert.-butyl carbonium ion, and then hydrolyzing the reaction mixture. Advantageously the acyl cyanide is pivaloyl cyanide or benzoyl cyanide and is reacted with an approximately equimolar amount of the ether in the presence of about 1.1 to 1.5 times the molar amount of concentrated sulphuric acid as the activating acid. The products are useful as intermediates in the synthesis of known herbicides.
    • 制备式R-CO-CO-NH-C(CH3)3的α-酮羧酸N-叔丁基酰胺的方法,其中R是具有至多8个碳原子的脂族基团,环烷基 具有3至6个碳原子,苯基或萘基或杂环基,其包括使式R-CO-CN的酰基氰与式(CH 3)3 C-O-CH 3的叔丁基甲基醚在 在能够在反应条件下活化式(III)的醚的酸存在下,温度在约0℃至80℃之间,得到叔丁基碳鎓离子,然后水解反应混合物。 有利地,酰基氰是新戊酰氰或苯甲酰氰,并且在作为活化酸的浓硫酸的摩尔量的约1.1至1.5倍的存在下,与约等摩尔量的醚反应。 该产品可用作合成已知除草剂的中间体。