The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of di...The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of diethylallylamine (DEAA), and drying and temperature on the synthesis of DEDAAC were investigated. The content of in-process product DEAA was determined by non-aqueous titration. The structure of product DEDAAC was identified with IR, 1 H NMR and elemental analysis. The results show that adding allyl chloride and sodium hydroxide alternately can increase the yield of DEAA and decrease by-products. In further synthesizing of DEDAAC from DEAA, the step of drying DEAA is very necessary. When DEAA is dried by solid sodium hydroxide, good columnar crystals with a high purity(mp 199.5-201.0 ℃) are obtained; when DEAA is undried or the content of water in DEAA is above 20%, only platelets with bad quality are obtained even without crystals. The suitable synthesis conditions for DEAA and DEDAAC are 35 ℃, 6 h and 40 ℃, 36 h, respectively, and their yields are 69.7% and 67.3%, respectively.展开更多
目的建立反相高效液相色谱(RP-HPLC)法,以测定肥儿散中甘草酸铵含量。方法色谱柱为Capcell PAK C18柱(250mm×4.6mm,5μm),流动相为乙腈-0.015mol/L磷酸(39∶61),流速为1.0mL/min,检测波长为250nm。结果甘草酸铵进样量在0.1732～2.0...目的建立反相高效液相色谱(RP-HPLC)法,以测定肥儿散中甘草酸铵含量。方法色谱柱为Capcell PAK C18柱(250mm×4.6mm,5μm),流动相为乙腈-0.015mol/L磷酸(39∶61),流速为1.0mL/min,检测波长为250nm。结果甘草酸铵进样量在0.1732～2.0784μg范围内与峰面积线性关系良好,r=1.0000,平均加样回收率为99.87%,RSD=1.2%。结论RP-HPLC法灵敏、简便,重现性好,结果准确,适用于肥儿散的质量控制。展开更多
文摘The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of diethylallylamine (DEAA), and drying and temperature on the synthesis of DEDAAC were investigated. The content of in-process product DEAA was determined by non-aqueous titration. The structure of product DEDAAC was identified with IR, 1 H NMR and elemental analysis. The results show that adding allyl chloride and sodium hydroxide alternately can increase the yield of DEAA and decrease by-products. In further synthesizing of DEDAAC from DEAA, the step of drying DEAA is very necessary. When DEAA is dried by solid sodium hydroxide, good columnar crystals with a high purity(mp 199.5-201.0 ℃) are obtained; when DEAA is undried or the content of water in DEAA is above 20%, only platelets with bad quality are obtained even without crystals. The suitable synthesis conditions for DEAA and DEDAAC are 35 ℃, 6 h and 40 ℃, 36 h, respectively, and their yields are 69.7% and 67.3%, respectively.
文摘目的建立反相高效液相色谱(RP-HPLC)法,以测定肥儿散中甘草酸铵含量。方法色谱柱为Capcell PAK C18柱(250mm×4.6mm,5μm),流动相为乙腈-0.015mol/L磷酸(39∶61),流速为1.0mL/min,检测波长为250nm。结果甘草酸铵进样量在0.1732～2.0784μg范围内与峰面积线性关系良好,r=1.0000,平均加样回收率为99.87%,RSD=1.2%。结论RP-HPLC法灵敏、简便,重现性好,结果准确,适用于肥儿散的质量控制。
