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PREPARATION METHOD OF THIOSALICYLIC ACID(OR 2-MERCAPTOBENZOIC ACID)

机译:硫代水杨酸(或2-巯基苯甲酸)的制备方法

摘要

PURPOSE: A preparation method of thiosalicylic acid by deoxidization-hydrolysis of 2-cyanobenzenesufonyl chloride and reduction-hydrolyzing is provided which increases yields of thiosalicylic acid without separate complicate purification process. CONSTITUTION: Thiosalicylic acid is prepared by reducing a compound(I) using zinc and acetic acid of 1: 4 - 1: 6 and hydrolyzing using water and hydrochloric acid of 1: 4 - 1: 6 at -10 to 130°C. For example, 2g 2-benzoic sulfimide and 3g phophorus pentachloride are melted in 15 ml solvent slowly, stirred for 10 min, added with 2g zinc chloride, reduced for 1 hr, cooled, added with ice water, extracted with chloroform or ether, and dried with anhydrous magnesium sulfate to give 2-cyanobenzenesufonyl chloride(yield 90%). The compound is useful as a precursor of thioxanthone in a photochemical field and a synthetic intermediate(syphon) in an agricultural chemical field.
机译:用途:提供了一种通过2-氰基苯磺酰氯的脱氧-水解和还原水解来制备硫代水杨酸的方法,该方法无需单独的复杂纯化过程即可提高硫代水杨酸的收率。组成:硫代水杨酸的制备方法是:使用锌和醋酸为1:4-1:6还原化合物(I),然后在-10至130℃下用水和盐酸为1:4-1:6水解。例如,将2g 2-苯甲硫酰亚胺和3g五氯化磷在15ml溶剂中缓慢融化,搅拌10分钟,加入2g氯化锌,还原1小时,冷却,加入冰水,用氯仿或乙醚萃取,然后用无水硫酸镁干燥,得到2-氰基苯磺酰氯(产率90%)。该化合物在光化学领域可用作噻吨酮的前体,在农业化学领域可用作合成中间体(虹吸管)。

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