碳酸钠作为一种非氮族碱,能高效促进芳亚甲基丙二腈和α-氟代酮的环丙烷化反应。在以碳酸钠为碱,1,4-二氧六环为溶剂,80℃条件下,反应能以62%~83%的产率合成顺式多取代环丙烷化合物。目标化合物的结构经1 H NMR,13 C NMR和MS确证。该方...碳酸钠作为一种非氮族碱,能高效促进芳亚甲基丙二腈和α-氟代酮的环丙烷化反应。在以碳酸钠为碱,1,4-二氧六环为溶剂,80℃条件下,反应能以62%~83%的产率合成顺式多取代环丙烷化合物。目标化合物的结构经1 H NMR,13 C NMR和MS确证。该方法具有反应条件温和,产率高和立体选择性高等特点。展开更多
A new biphenol-like monomer,4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] was synthesized from phthalic anhydride and diphenylmethane in two steps.In the first step,Friedel-Crafts reaction was carried out...A new biphenol-like monomer,4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] was synthesized from phthalic anhydride and diphenylmethane in two steps.In the first step,Friedel-Crafts reaction was carried out in 1,2-dichloroethane between diphenylmethane and phthalic anhydride.The obtained product was used in the second step with hydrazine monohydrate added into its solution,followed by recrystallization in acetic acid.The melting point showed by differential scanning calorimetry of the bis(phthalazinone) monomer was 338.1℃.The overall yield of the biphenol-like monomer was 60%.A new polyphthalazinone was prepared from 4,4′-difluorodiphenylketone(DFK) and 4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] by solution polycondensation in N-methyl-2-pyrrolidone(NMP) with anhydrous K 2CO 3 as a catalyst.High molecular weight polymer was formed in 8 h at 190℃.The polymer was refined by precipitation from its 15% NMP solution with methanol as the precipitating agent.The powder of the polymer was dried in a vacuum oven under 120℃ for 48*!h and then under 200℃ for 4*!h.The intrinsic viscosity of the polymer was 0.58*!dL/g in NMP at 25℃.The polymer showed high glass transition temperature (T g) at 258℃ by DSC.The decomposition temperature for 5% weight loss (T d5) in nitrogen measured by thermogravimetric analysis occurred at 431℃.The solubility of the polymer was investigated at room temperature.The polymer was soluble in NMP,m-cresol and partially soluble in chloroform,and insoluble in N,N-dimethylacetamide (DMAc) and dimethyl sulfoxide (DMSO).The methylene group and bis-(phthalazinone) structure in the backbone of the polymer contribute much to the good solubility,and the rigid structure of bis(phthalazinone) retains its good thermal properties.展开更多
目的建立卡西酮、甲卡西酮、4-甲基甲卡西酮的LC-MS/MS定性定量分析方法。方法采用Agilent6460三重串联四极杆液质联用仪(LC/QQQ),样品用甲醇直接提取,采用Agilent Zorbax○R Eclipse Plus C18色谱柱(100mm×2.1mm,1.8μm),流动相为...目的建立卡西酮、甲卡西酮、4-甲基甲卡西酮的LC-MS/MS定性定量分析方法。方法采用Agilent6460三重串联四极杆液质联用仪(LC/QQQ),样品用甲醇直接提取,采用Agilent Zorbax○R Eclipse Plus C18色谱柱(100mm×2.1mm,1.8μm),流动相为0.1%甲酸和乙腈,梯度洗脱,流速为0.3mL/min,进样体积为3μL。质谱应用ESI源、正离子模式、多反应监测(MRM)方式检测卡西酮、甲卡西酮、4-甲基甲卡西酮。结果卡西酮的线性范围为1ng/mL^25000ng/mL,甲卡西酮的线性范围为0.1ng/mL^10000ng/mL,4-甲基甲卡西酮的线性范围为1ng/mL^10000ng/mL。结论该方法简单、准确,灵敏度高,可以满足案件鉴定工作的需要。展开更多
文摘碳酸钠作为一种非氮族碱,能高效促进芳亚甲基丙二腈和α-氟代酮的环丙烷化反应。在以碳酸钠为碱,1,4-二氧六环为溶剂,80℃条件下,反应能以62%~83%的产率合成顺式多取代环丙烷化合物。目标化合物的结构经1 H NMR,13 C NMR和MS确证。该方法具有反应条件温和,产率高和立体选择性高等特点。
文摘A new biphenol-like monomer,4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] was synthesized from phthalic anhydride and diphenylmethane in two steps.In the first step,Friedel-Crafts reaction was carried out in 1,2-dichloroethane between diphenylmethane and phthalic anhydride.The obtained product was used in the second step with hydrazine monohydrate added into its solution,followed by recrystallization in acetic acid.The melting point showed by differential scanning calorimetry of the bis(phthalazinone) monomer was 338.1℃.The overall yield of the biphenol-like monomer was 60%.A new polyphthalazinone was prepared from 4,4′-difluorodiphenylketone(DFK) and 4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] by solution polycondensation in N-methyl-2-pyrrolidone(NMP) with anhydrous K 2CO 3 as a catalyst.High molecular weight polymer was formed in 8 h at 190℃.The polymer was refined by precipitation from its 15% NMP solution with methanol as the precipitating agent.The powder of the polymer was dried in a vacuum oven under 120℃ for 48*!h and then under 200℃ for 4*!h.The intrinsic viscosity of the polymer was 0.58*!dL/g in NMP at 25℃.The polymer showed high glass transition temperature (T g) at 258℃ by DSC.The decomposition temperature for 5% weight loss (T d5) in nitrogen measured by thermogravimetric analysis occurred at 431℃.The solubility of the polymer was investigated at room temperature.The polymer was soluble in NMP,m-cresol and partially soluble in chloroform,and insoluble in N,N-dimethylacetamide (DMAc) and dimethyl sulfoxide (DMSO).The methylene group and bis-(phthalazinone) structure in the backbone of the polymer contribute much to the good solubility,and the rigid structure of bis(phthalazinone) retains its good thermal properties.
文摘目的建立卡西酮、甲卡西酮、4-甲基甲卡西酮的LC-MS/MS定性定量分析方法。方法采用Agilent6460三重串联四极杆液质联用仪(LC/QQQ),样品用甲醇直接提取,采用Agilent Zorbax○R Eclipse Plus C18色谱柱(100mm×2.1mm,1.8μm),流动相为0.1%甲酸和乙腈,梯度洗脱,流速为0.3mL/min,进样体积为3μL。质谱应用ESI源、正离子模式、多反应监测(MRM)方式检测卡西酮、甲卡西酮、4-甲基甲卡西酮。结果卡西酮的线性范围为1ng/mL^25000ng/mL,甲卡西酮的线性范围为0.1ng/mL^10000ng/mL,4-甲基甲卡西酮的线性范围为1ng/mL^10000ng/mL。结论该方法简单、准确,灵敏度高,可以满足案件鉴定工作的需要。
