山西化工
山西化工
산서화공
SHANXI CHEMICAL INDUSTRY
2012年
4期
1-4
,共4页
4-硝基咪唑%单因素实验%合成
4-硝基咪唑%單因素實驗%閤成
4-초기미서%단인소실험%합성
4-nitroimidazoles%single factor experiment%synthesis
探讨了合成4-硝基咪唑的方法以及如何提高其得率的问题。对样品进行了熔点测定,采用红外光谱进行了表征,验证了所得反应产物。通过单因素实验得出最佳操作条件：咪唑酸化时间40 min,温度控制在25℃以下;硝硫混酸硝化硫酸咪唑盐时间2.5 h,控制温度55℃;在冰点附近调节反应液的pH=3～4,然后进行减压蒸馏抽滤,可以使产物最大限度地析出。
探討瞭閤成4-硝基咪唑的方法以及如何提高其得率的問題。對樣品進行瞭鎔點測定,採用紅外光譜進行瞭錶徵,驗證瞭所得反應產物。通過單因素實驗得齣最佳操作條件：咪唑痠化時間40 min,溫度控製在25℃以下;硝硫混痠硝化硫痠咪唑鹽時間2.5 h,控製溫度55℃;在冰點附近調節反應液的pH=3～4,然後進行減壓蒸餾抽濾,可以使產物最大限度地析齣。
탐토료합성4-초기미서적방법이급여하제고기득솔적문제。대양품진행료용점측정,채용홍외광보진행료표정,험증료소득반응산물。통과단인소실험득출최가조작조건：미서산화시간40 min,온도공제재25℃이하;초류혼산초화류산미서염시간2.5 h,공제온도55℃;재빙점부근조절반응액적pH=3～4,연후진행감압증류추려,가이사산물최대한도지석출。
This article discusses the synthesis of 4-nitroimidazole method, and how to improve its yield problems. The melting point of the samples was measured; and the infrared spectroscopy was used to characterize, The results of characterization shows that the reaction product obtained was target compound. Through the single factor experiment, the conclusions are as follows: the optimal operating conditions were :acidifieation time 40 min under the temperature of 25℃ ; nitric-sulfuric acid nitration acid imidazole salt time 2.5 h, control temperature at 55 ℃ ; in the near freezing point regulation of pH of reaction solution to 3 - 4, and then reducing pressure distillation, filtration, it can obtain the products of maximum precipitation.
