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CN102557995A N-乙氧甲酰基-5-氯-2-甲基-4-氨磺酰基苯胺的合成方法 无效 - 撤回

N-乙氧甲酰基-5-氯-2-甲基-4-氨磺酰基苯胺的合成方法
摘要：
本发明涉及美托拉宗中间体(II)-N-乙氧甲酰基-5-氯-2-甲基-4-氨磺酰基苯胺的制备方法。它是以N-乙氧甲酰基-5-氯-2-甲基-苯胺、氯磺酸为原料，使用氯化亚砜为溶剂进行反应，步骤为：将氯磺酸加入干燥的反应器中，搅拌状态下加入N-乙氧甲酰基-5-氯-2-甲基-苯胺，加热，保温10-14小时。然后加入氯化亚砜。继续保温10-14小时；最后经冰解、氨化、过滤。本发明通过加入氯化亚砜能有效避免因氯磺酸含量不同对本反应产生的影响，同时减少氯磺酸的用量，是一种更加有效地提高美托拉宗中间体(II)-N-乙氧甲酰基-5-氯-2-甲基-4-氨磺酰基苯胺的收率和质量的制备方法。
摘要（英）：

The invention relates to a method for preparing N-ethoxalyl-5-choro-2-methyl-4-sulfanoyl aniline, namely metolazone intermediate (II). According to the method, N-ethoxalyl-5-choro-2-methyl-aniline and chlorosulfonic acid are used as raw materials, and thionyl chloride is used as a solvent for reaction. The method comprises the following steps of: adding chlorosulfonic acid into a dried reactor, adding N-ethoxalyl-5-choro-2-methyl-aniline with stirring, heating, and preserving heat for 10 to 14 hours; adding thionyl chloride; continuously preserving heat for 10 to 14 hours; and performing calving and ammoniation and filtering. By adding thionyl chloride, the influence caused by different content of chlorosulfonic acid on the reaction can be effectively avoided; the using amount of chlorosulfonic acid is reduced; and by the method for preparing N-ethoxalyl-5-choro-2-methyl-4-sulfanoyl aniline, namely metolazone intermediate (II), yield and quality of N-ethoxalyl-5-choro-2-methyl-4-sulfanoyl aniline are improved effectively.

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