广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2014年
11期
66-67
,共2页
N-芳基哌嗪%二氯乙胺盐酸盐%取代苯胺%合成工艺
N-芳基哌嗪%二氯乙胺鹽痠鹽%取代苯胺%閤成工藝
N-방기고진%이록을알염산염%취대분알%합성공예
N-aryl piperazines%N,N-bis ( 2 -chloroethyl ) amine hydrochloride%substituted aniline%synthetic process
以二氯乙胺盐酸盐和取代苯胺为原料,正丁醇做溶剂,在无碱的条件下回流以较高产率合成了取代芳基哌嗪,其结构经1 H-NMR确认无误。由于反应产物能直接从反应体系中结晶析出且滤液可重复套用多次,使得该合成新方法适合于工业化规模生产。与文献报道方法相比较,新工艺简化了操作步骤、降低了产物的分离难度、提高了收率和产品纯度。
以二氯乙胺鹽痠鹽和取代苯胺為原料,正丁醇做溶劑,在無堿的條件下迴流以較高產率閤成瞭取代芳基哌嗪,其結構經1 H-NMR確認無誤。由于反應產物能直接從反應體繫中結晶析齣且濾液可重複套用多次,使得該閤成新方法適閤于工業化規模生產。與文獻報道方法相比較,新工藝簡化瞭操作步驟、降低瞭產物的分離難度、提高瞭收率和產品純度。
이이록을알염산염화취대분알위원료,정정순주용제,재무감적조건하회류이교고산솔합성료취대방기고진,기결구경1 H-NMR학인무오。유우반응산물능직접종반응체계중결정석출차려액가중복투용다차,사득해합성신방법괄합우공업화규모생산。여문헌보도방법상비교,신공예간화료조작보취、강저료산물적분리난도、제고료수솔화산품순도。
By using N,N-bis(2-chloroethyl)amine hydrochloride and substituted aniline as initial material , n-butyl alcohol as the solvent , refluxing in the absence of base to convert to corresponding N -aryl piperazines in high yield.The structure was confirmed by 1 H-NMR.The product can crystallize directly from the system and the filtrate can be used several times so that the new synthetic method was applicable in the industrial scale production .Compared to the reported method , the new process simplified the operation steps , reduced the difficulty of the product separation and improved the yield and purity of the product.