印染助剂
印染助劑
인염조제
TEXTILE AUXILIARIES
2014年
9期
16-19
,共4页
王丽艳%孙雷%秦红磊%佟白%张超%孟令威%陆强娜
王麗豔%孫雷%秦紅磊%佟白%張超%孟令威%陸彊娜
왕려염%손뢰%진홍뢰%동백%장초%맹령위%륙강나
2-氧代-2,3-二氢-1H-咪唑并1,2-a-吡啶鎓氯化物%单因素试验%合成%表征
2-氧代-2,3-二氫-1H-咪唑併1,2-a-吡啶鎓氯化物%單因素試驗%閤成%錶徵
2-양대-2,3-이경-1H-미서병1,2-a-필정옹록화물%단인소시험%합성%표정
2-oxo-2,3-dihydro-1H-imidazo[1,2-a]-pyridinium chloride%single factor experiment%syn-thesis%characterization
以2-氨基吡啶和氯乙酰氯为原料,合成2-(2-氯乙酰氨基)吡啶,进一步环合生成2-氧代-2,3-二氢-1H-咪唑并[1,2-a]-吡啶鎓氯化物.分别考察物质的量比、反应温度、反应时间对中间体及目标产物收率的影响.通过单因素试验,确定合成2-(2-氯乙酰氨基)吡啶的较佳工艺条件为:氯仿为溶剂,反应温度0℃,反应时间4 h,n(2-氨基吡啶)∶n(氯乙酰氯)=1∶1.5;合成2-氧代-2,3-二氢-1H-咪唑并[1,2-a]-吡啶鎓氯化物的较佳工艺条件为:乙腈为溶剂,反应温度75℃,反应时间12 h.利用1H-NMR和IR对中间体及目标产物结构进行了表征.
以2-氨基吡啶和氯乙酰氯為原料,閤成2-(2-氯乙酰氨基)吡啶,進一步環閤生成2-氧代-2,3-二氫-1H-咪唑併[1,2-a]-吡啶鎓氯化物.分彆攷察物質的量比、反應溫度、反應時間對中間體及目標產物收率的影響.通過單因素試驗,確定閤成2-(2-氯乙酰氨基)吡啶的較佳工藝條件為:氯倣為溶劑,反應溫度0℃,反應時間4 h,n(2-氨基吡啶)∶n(氯乙酰氯)=1∶1.5;閤成2-氧代-2,3-二氫-1H-咪唑併[1,2-a]-吡啶鎓氯化物的較佳工藝條件為:乙腈為溶劑,反應溫度75℃,反應時間12 h.利用1H-NMR和IR對中間體及目標產物結構進行瞭錶徵.
이2-안기필정화록을선록위원료,합성2-(2-록을선안기)필정,진일보배합생성2-양대-2,3-이경-1H-미서병[1,2-a]-필정옹록화물.분별고찰물질적량비、반응온도、반응시간대중간체급목표산물수솔적영향.통과단인소시험,학정합성2-(2-록을선안기)필정적교가공예조건위:록방위용제,반응온도0℃,반응시간4 h,n(2-안기필정)∶n(록을선록)=1∶1.5;합성2-양대-2,3-이경-1H-미서병[1,2-a]-필정옹록화물적교가공예조건위:을정위용제,반응온도75℃,반응시간12 h.이용1H-NMR화IR대중간체급목표산물결구진행료표정.
2-(2-chloro-acetylamino) pyridine was synthesized with 2-aminopyridine and chloroacetyl chloride, and then 2-oxo-2,3-dihydro-1H-imidazo[1,2-a]-pyridinium chloride was synthesized through cycli-zation reaction. The influences of molar ratio, reaction temperature and time on the yield of intermediate and product were investigated. The synthesis processes of 2-(2-chloro-acetylamino) pyridine and 2-oxo-2,3-di-hydro-1H-imidazo[1,2-a]-pyridinium chloride were determined through the single factor experiment. The opti-mal synthesis process of 2-(2-chloro-acetylamino) pyridine was as fol ows: the chloroform as solvent, react-ed at 0 ℃ for 4 h, the molar ratio of 2-aminopyridine to chloroacetyl chloride was 1∶1.5. The optimal synthe-sis process of 2-oxo-2,3-dihydro-1H-imidazo[1,2-a]-pyridinium chloride was as fol ows: the acetonitrile as solvent, reacted at 75℃for 12 h. The product was characterized by IR and 1H-NMR.