Novel synthesis technology of N-methyl-2-methyl-3-thia-5-chlorovaleryl amine

A process for synthesizing N-methyl-2-methyl-3-thia-5-chloropentylamide includes such steps as heating chloropropionate to 50-60 deg.C, adding methanol solution of methylamine, reaction for 1-2 hr, distilling to removing methanol, adding methanol solution of sodium carboxyl ethoxide, reaction at 50-...

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Main Authors JINQING HAN, YUANAN JIA, YIMIN MA
Format Patent
LanguageChinese
English
Published 22.12.2004
Edition7
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Abstract A process for synthesizing N-methyl-2-methyl-3-thia-5-chloropentylamide includes such steps as heating chloropropionate to 50-60 deg.C, adding methanol solution of methylamine, reaction for 1-2 hr, distilling to removing methanol, adding methanol solution of sodium carboxyl ethoxide, reaction at 50-60 deg.C for 2 hr, filtering out sodium chloride, distilling out methanol, adding trichloromethane, dripping sulfoxide chloride, and reaction for 2 hr. N-甲基-2-甲基-3-硫杂-5-氯戊酰胺的一种合成工艺,其特征是包括以下步骤:1.将氯丙酸酯加热到50-60℃,加一甲胺甲醇溶液,反应1-2小时,蒸出溶剂甲醇;2.加入巯基乙醇钠的甲醇溶液,在50-60℃反应2小时,然后过滤出去氯化钠,蒸出溶剂甲醇;3.加入三氯甲烷,在温度0-5℃下滴加氯化亚砜,室温反应2小时;本发明减去了加固体氢氧化钠的麻烦,温度易控制,反应平稳,目标化合物不易分解,收率高,产品含量达到95%以上,有利其高含量衍生物的生成;并且减少原料消耗,节约了能源,降低了成本。
AbstractList A process for synthesizing N-methyl-2-methyl-3-thia-5-chloropentylamide includes such steps as heating chloropropionate to 50-60 deg.C, adding methanol solution of methylamine, reaction for 1-2 hr, distilling to removing methanol, adding methanol solution of sodium carboxyl ethoxide, reaction at 50-60 deg.C for 2 hr, filtering out sodium chloride, distilling out methanol, adding trichloromethane, dripping sulfoxide chloride, and reaction for 2 hr. N-甲基-2-甲基-3-硫杂-5-氯戊酰胺的一种合成工艺,其特征是包括以下步骤:1.将氯丙酸酯加热到50-60℃,加一甲胺甲醇溶液,反应1-2小时,蒸出溶剂甲醇;2.加入巯基乙醇钠的甲醇溶液,在50-60℃反应2小时,然后过滤出去氯化钠,蒸出溶剂甲醇;3.加入三氯甲烷,在温度0-5℃下滴加氯化亚砜,室温反应2小时;本发明减去了加固体氢氧化钠的麻烦,温度易控制,反应平稳,目标化合物不易分解,收率高,产品含量达到95%以上,有利其高含量衍生物的生成;并且减少原料消耗,节约了能源,降低了成本。
Author YUANAN JIA
JINQING HAN
YIMIN MA
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Snippet A process for synthesizing N-methyl-2-methyl-3-thia-5-chloropentylamide includes such steps as heating chloropropionate to 50-60 deg.C, adding methanol...
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Title Novel synthesis technology of N-methyl-2-methyl-3-thia-5-chlorovaleryl amine
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