基于串联反应的吡虫啉新合成工艺研究

以2-氯-5-氯甲基吡啶(CCMP)、无水乙二胺和硝基胍为原料,运用串联反应方法合成了吡虫啉[化学名:1-(6-氯-3-吡啶甲基)-N-硝基-2-咪唑啉亚胺]。该方法反应中间体无需纯化处理,操作简单,同时解决了活性中间体进一步进行副反应的难题。通过单因素实验,探讨了pH、反应溶剂、温度以及时间等因素对产物收率的影响,得到的优化工艺条件为:以乙腈为溶剂,nCCMP∶n无水乙二胺∶n硝基胍=1∶5∶1,于30℃反应120min,产率可达96.35%。其结构经1H NMR、13C NMR、IR表征。     

基于串联反应的吡虫啉新合成工艺研究

以2-氯-5-氯甲基吡啶(CCMP)、无水乙二胺和硝基胍为原料,运用串联反应方法合成了吡虫啉[化学名:1-(6-氯-3-吡啶甲基)-N-硝基-2-咪唑啉亚胺]。该方法反应中间体无需纯化处理,操作简单,同时解决了活性中间体进一步进行副反应的难题。通过单因素实验,探讨了pH、反应溶剂、温度以及时间等因素对产物收率的影响,得到的优化工艺条件为:以乙腈为溶剂,nCCMP∶n无水乙二胺∶n硝基胍=1∶5∶1,于30℃反应120min,产率可达96.35%。其结构经1H NMR、13C NMR、IR表征。     

Dielectric Performance of Porous Methyl Silsesquioxane/Triacetyl-β-Cyclodextrin Thin Films

Porous methyl silsesquioxane thin films with low dielectric constant are successfully synthesized by means of the sol-gel spin-coating method. The precursor solutions are prepared by properly mixing the polymer as a matrix with different contents of triacetyl-β-cyclodextrin （TABCD） as a porogen. The chemical structure, dielectric constants, optical constants and void fraction are investigated by the ellipsometric porosimetry, Fourier transform infrared （FTIR） spectroscopy, and other methods. Influences of TABCD and methyl trimethoxysilane （MTMS） on the dielectric properties are discussed. For those samples with higher porogen loading, orientation and electronic polarizations are lower in low and high frequency regions, respectively, because of a considerably smaller number of polar molecules. The FTIR results suggest that high R value （molar ratio of H2 O to MTMS） is more advantageous for formation of cage structures and the cage/network structural ratio increases with the increasing R value.     

Experimental demonstration of narrow-band rugate minus filters using rapidly alternating deposition technology

The design, fabrication and performance of narrow-band rugate minus filters are investigated in this paper. A method of fabricating graded-index coatings by rapidly alternating deposition of low(Si O2) and high(Al2 O3) refractive index materials is presented to fabricate a rugate structure. The narrow-band rugate minus filter design and fabrication approaches are discussed in detail. The experimental results, including transmittance spectrum, surface damage test and damage morphology investigated with a scanning electron microscope, demonstrate the high performance of the as-fabricated spatial filter and confirm the feasibility of the fabrication method for narrow-band rugate minus filters.