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PROCESS FOR THE SYNTHESIS OF N-AMINO AZA-3 BICYCLO 3,3, O-OCTANE

机译:N-氨基氮杂AZA-3 Bicyclo的合成过程] 3,3,O-辛烷

摘要

1. A process for continuous synthesis of N-amino-3-aza-bicyclo[3,3,0]octane characterized by reacting a solution of ammonium hydroxide and ammonium chloride with an aqueous solution of sodium hypochlorite at a temperature between -15 degrees C and -7 degrees C in an alkaline medium, - then reacting the thus formed monochloroamine with 3-aza-bicyclo[3,3,0]octane in a two-phase medium in a suitable reaction vessel equipped with a blade agitator at a temperature between 30 degrees C and 90 degrees C in an alkaline medium, - then separating by destillation the ammonia and subsequent the non-reacted 3-aza-bicyclo[3,3,0]octane from the reaction medium for recycling, - then isolating under demixing a concentrated solution of N-amino-3-aza-bicyclo[3,3,0]octane by addition of sodium hydroxide to the reaction medium and, if desired, purifying the thus formed hydrazine by destillation.
机译:1.连续合成N-氨基-3-氮杂双环[3,3,0]辛烷的方法,其特征在于使氢氧化铵和氯化铵的溶液与次氯酸钠水溶液在-15度之间的温度反应碱性介质中在摄氏零下(7和7摄氏度),然后在两相介质中,在装有叶片搅拌器的合适反应容器中,将如此形成的一氯胺与3-氮杂-双环[3,3,0]辛烷在两相介质中反应。在碱性介质中的30摄氏度至90摄氏度之间的温度下,-然后通过蒸馏将氨和随后未反应的3-氮杂双环[3,3,0]辛烷从反应介质中蒸馏出来以进行再循环,-然后进行分离在将N-氨基-3-氮杂-双环[3,3,0]辛烷的浓缩溶液中通过向反应介质中加入氢氧化钠进行混合,并且如果需要的话,通过蒸馏来纯化由此形成的肼。

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