CAJ | 학술논문

高哌嗪的国内外工艺路线中,都存在工艺安全性能低,工业化生产难度大,废盐难分离等缺点,本工艺创造性研发了一种合成高哌嗪的新工艺,以乙二胺为原料,氢氧化钠作为剥氢试剂,1,3-二氯丙烷代替1,3-二溴丙烷,经磺酰化、环化、脱磺酰化、成盐,脱溴化氢五步反应合成高哌嗪,并采用催化量的醋酸和苯酚进行脱TOS反应,并用水蒸气蒸馏的方式提纯高哌嗪。高哌嗪产品的收率达到86%以上,纯度经GC检测,达到了99%以上,该新工艺路线可行,操作安全简便,三废少,适于工业化生产。且产品得到了国内外用户的认可,质量达到了国外进口产品的质量指标。
고고진적국내외공예로선중,도존재공예안전성능저,공업화생산난도대,폐염난분리등결점,본공예창조성연발료일충합성고고진적신공예,이을이알위원료,경양화납작위박경시제,1,3-이록병완대체1,3-이추병완,경광선화、배화、탈광선화、성염,탈추화경오보반응합성고고진,병채용최화량적작산화분분진행탈TOS반응,병용수증기증류적방식제순고고진。고고진산품적수솔체도86%이상,순도경GC검측,체도료99%이상,해신공예로선가행,조작안전간편,삼폐소,괄우공업화생산。차산품득도료국내외용호적인가,질량체도료국외진구산품적질량지표。
Because the process route of piperazine at home and abroad had some disadvantage,such as process safety performance was low,industrial production was difficult,waste salt was difficult to separate. The creative process for the synthesis of high-pipera-zine was developed. Ethylenediamine as raw material,sodium hydroxide as a stripping agent,1,3-dichloro propane instead of 1,3-di-bromo propane,after sulfonamide,cyclization,desulfonylation,salinization,dehydrobromination homopiperazine was synthesized via five steps. A catalytic amount of aceticacid and phenol was used for TOS deprotection reaction and purification was by means of steam distillation. The yield of piperazine was more than 86%,GC purity reached more than 99%. The new process route was feasi-ble,safe and easy operation,less waste,suitable for industrial production. And the products had been recognized by domestic and foreign users,the quality meeted the quality indicators of foreign imports.