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Griseofulvin (GF) is an antifungal drug whose pharmaceutical activity can be improved by reducing particle size. In this study the rapid expansion of supercritical solution (RESS) was employed to micronize GF.Carbon dioxide with cosolvent acetone was chosen as a supercritical mixed solvent. The solubility of GF in super-critical CO2 with cosolvent acetone was measured using a dynamic apparatus at pressures between 12 and 32 MPa,temperatures at 313, 323 and 333 K and cosolvent concentration at 1.5, 3.0, 4.5 and 6.0% (by mole). The effect of pre-expansion pressure, extraction temperature, spraying distance, nozzle size and concentration of cosolvent on the precipitated particles was investigated. The results show that the mean particle size of griseofulvin precipitated by RESS was less than 1.2μm. An increase in pre-expansion pressure, extraction temperature, spraying distance and concentration of cosolvent resulted in a decrease in particle size under the operating condition studied. With the decrease of nozzle diameter the particle size reduces. The crystallinity and melting point of the original material and the processed particle by RESS were tested by X-ray diffraction (XRD) and differential scanning calorimetry (DSC).No evident modification in the crystal habit was found under the experimental conditions tested. The morphology of particles precipitated was analyzed bY scanning electron microscopy (SEM). 相似文献
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摘 要 本文采用正丁醇、多聚甲醛及干燥的氯化氢气体为主要原料,合成氯甲基化试剂烷基氯甲醚-氯甲氧基丁烷(CMB)。采用红外光谱(FTIR)与核磁共振谱(1H-NMR)对产物进行了表征。考察了溶剂用量,物料摩尔比,反应温度及反应时间对CMB收率的影响。采用正交试验法获得的最佳反应条件为溶剂1,2-二氯乙烷50 mL,n(正丁醇):n(CH2O)=3:2.00, 温度为0-5 ℃, 反应时间为7 h。在此条件下,氯甲氧基丁烷的收率可达92%。用制备的氯甲氧基丁烷氯甲基化交联度为10%的白球,用佛尔哈德滴定法测氯含量,测得制得氯球中氯含量为13%。 相似文献
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以N-(喹啉-8-基)新戊酰胺和DL-1-苯乙醇为原料,酸酐为添加剂,无水三氯化铁为催化剂,1,2-二氯乙烷为溶剂制备标题化合物,产品结构经1HNMR和13CNMR表征。通过单因素实验,考察添加剂的种类、反应时间、反应温度、催化剂用量、添加剂用量对反应收率的影响,最终确定合成标题化合物的最佳条件为:n(N-(喹啉-8-基)新戊酰胺)∶n(DL-1-苯乙醇)∶n(添加剂)=1∶3∶3,催化剂为20 mol%无水三氯化铁,溶剂为1,2-二氯乙烷,反应温度为140℃、反应时间为24 h,产品收率可达83%。方法原料易得、操作简单、步骤节省,为产品的工业化奠定了基础。 相似文献
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Griseofulvin (GF) is an antifungal drug whose pharmaceutical activity can be improved by reducingparticle size. In this study the rapid expansion of supercritical solution (RESS) was employed to micronize GF.Carbon dioxide with cosolvent acetone was chosen as a supercritical mixed solvent. The solubility of GF in super-critical CO2 with cosolvent acetone was measured using a dynamic apparatus at pressures between 12 and 32 MPa,temperatures at 313, 323 and 333K and cosolvent concentration at 1.5, 3.0, 4.5 and 6.0% (by mole). The effect ofpre-expansion pressure, extraction temperature, spraying distance, nozzle size and concentration of cosolvent on theprecipitated particles was investigated. The results show that the mean particle size of griseofulvin precipitated byRESS was less than 1.2 μm. An increase in pre-expansion pressure, extraction temperature, spraying distance andconcentration of cosolvent resulted in a decrease in particle size under the operating condition studied. With thedecrease of nozzle diameter the particle size reduces. The crystallinity and melting point of the original material andthe processed particle by RESS were tested by X-ray diffraction (XRD) and differential scanning calorimetry (DSC).No evident modification in the crystal habit was found under the experimental conditions tested. The morphologyof particles precipitated was analyzed by scanning electron microscopy (SEM). 相似文献
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氯甲氧基丁烷的制备及初步应用 总被引:1,自引:1,他引:0
用正丁醇、多聚甲醛及干燥的氯化氢气体为主要原料,合成氯甲基化试剂———氯甲氧基丁烷(CMB)。采用傅里叶变换红外光谱(FTIR)与核磁共振氢谱(1HNMR)对产物进行了表征。考察了溶剂用量、物料摩尔比、反应温度及反应时间对CMB收率的影响。获得的最佳反应条件为:溶剂1,2-二氯乙烷50 mL,n(正丁醇)∶n(多聚甲醛)=3∶2,温度为0~5℃,反应时间为7 h;在该条件下,氯甲氧基丁烷的收率可达92%。用制备的氯甲氧基丁烷氯甲基化交联度为10%的白球得到氯甲基化聚苯乙烯微球,并用佛尔哈德滴定法测得其中氯的质量分数为13%。 相似文献
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