目的:用高效液相法同时测定山楂叶中牡荆素-4〃-O-葡萄糖苷、牡荆素鼠李糖苷、牡荆素、芦丁、金丝桃苷的含量。方法:采用HPLC法,色谱柱:Sepax HP C18柱(4.6 mm×250mm,5μm);流动相:A为乙腈-四氢呋喃(20:1),B为0.5%甲酸溶液,采用梯...目的:用高效液相法同时测定山楂叶中牡荆素-4〃-O-葡萄糖苷、牡荆素鼠李糖苷、牡荆素、芦丁、金丝桃苷的含量。方法:采用HPLC法,色谱柱:Sepax HP C18柱(4.6 mm×250mm,5μm);流动相:A为乙腈-四氢呋喃(20:1),B为0.5%甲酸溶液,采用梯度洗脱;0～10min,A为14%～17%;10～26min,A为17%～18%;26～28min,A为18%～14%;检测波长:360nm,流速:1.0mL/min;柱温:32℃。结果:该方法加样回收率牡荆素-4″-O-葡萄糖苷:99.59%(RSD=0.50%),牡荆素鼠李糖苷:99.57%(RSD=0.96%),牡荆素:98.70%(RSD=1.10%),芦丁:99.35%(RSD=1.16%),金丝桃苷:99.28%(RSD=0.88%)。结论:该方法准确可靠,重现性好,可用于山楂叶的质量控制。展开更多
This paper reports that in the presence of cetyltrimethyl ammonium bromide as phase transfer catalyst,D-glucosamine hydrochloride reacts with 2,4-dinitrophenol to synthesize 1-O-(2’,4’-dinitrophenyl)-2-acetamido-β-...This paper reports that in the presence of cetyltrimethyl ammonium bromide as phase transfer catalyst,D-glucosamine hydrochloride reacts with 2,4-dinitrophenol to synthesize 1-O-(2’,4’-dinitrophenyl)-2-acetamido-β-D-glucoside.Chemical structure of the new compound was confirmed by elemental analysis,IR and UV.展开更多
Four pyridazinone gluosodes 4 were synthesized by Koenig′s Knorr reaction of 6 (4 halophenyl) 3( 2H ) pyridazinone silver salt 2 with bromoacetylglucose 3.Treatment of 4 with dry ammonia at 0～-5℃ effected a removal...Four pyridazinone gluosodes 4 were synthesized by Koenig′s Knorr reaction of 6 (4 halophenyl) 3( 2H ) pyridazinone silver salt 2 with bromoacetylglucose 3.Treatment of 4 with dry ammonia at 0～-5℃ effected a removal of the acetyl protecting groups to yield compounds 5.When the substituent on the benaene ring was F or Cl ,O glucoside was synthesized principally.However,when the substituent was Br or I ,N glucoside was mainly obtained.Their structures were confirmed by 1H NMR,IR and elemental analysis.展开更多
为克服目前合成方法存在收率较低,反应时间长、产品分离困难等不足,本文以β-D-葡萄糖、乙酰溴为原料,经乙酰化、溴代反应合成了糖基体2,3,4,6-O-四乙酰基-α-D-溴代葡萄糖,再与4-羟基苯甲醛衍生物经糖苷化反应合成了5种4-甲酰基苯基(2,...为克服目前合成方法存在收率较低,反应时间长、产品分离困难等不足,本文以β-D-葡萄糖、乙酰溴为原料,经乙酰化、溴代反应合成了糖基体2,3,4,6-O-四乙酰基-α-D-溴代葡萄糖,再与4-羟基苯甲醛衍生物经糖苷化反应合成了5种4-甲酰基苯基(2,3,4,6-O-四乙酰基)-β-D-葡萄糖苷衍生物。在合成4-甲酰基苯基(2,3,4,6-O-四乙酰基)-β-D-葡萄糖苷衍生物的过程中,采用10%(质量分数) Na OH溶液为缚酸剂,三(3,6-二氧杂庚基)胺(TDA-1)为相转移催化剂,反应物的收率为61%～69%,并应用核磁共振技术确定了产品的结构。该方法具有产品收率较高,反应温和、操作简单等优点。展开更多
Starting from \%D\%\|galactose, per\|\%O\|\%acetylated (\%S\%)\|TBMB carboxylic acid derivant of methyl\|4\|amino\|4\|deoxy\|\%D\%\|glucopyranoside was prepared. The mechanism of the possible side reactions of the cat...Starting from \%D\%\|galactose, per\|\%O\|\%acetylated (\%S\%)\|TBMB carboxylic acid derivant of methyl\|4\|amino\|4\|deoxy\|\%D\%\|glucopyranoside was prepared. The mechanism of the possible side reactions of the catalytic reduction from different types of azide sugar to the corresponding amino sugar was discussed. 1\|\%O\%\|Me\|protection was selected for preventing the intramolecular dehydration of the 4\|amino sugar, which was a key intermediate product in this synthetic process. The product was characterized by HRMS and \{\{\}\+1H NMR\} spectroscopy and will be used as a molecular model to develop a new identification method of the \%D, L\|\%configurations of amino sugar.展开更多
文摘目的:用高效液相法同时测定山楂叶中牡荆素-4〃-O-葡萄糖苷、牡荆素鼠李糖苷、牡荆素、芦丁、金丝桃苷的含量。方法:采用HPLC法,色谱柱:Sepax HP C18柱(4.6 mm×250mm,5μm);流动相:A为乙腈-四氢呋喃(20:1),B为0.5%甲酸溶液,采用梯度洗脱;0～10min,A为14%～17%;10～26min,A为17%～18%;26～28min,A为18%～14%;检测波长:360nm,流速:1.0mL/min;柱温:32℃。结果:该方法加样回收率牡荆素-4″-O-葡萄糖苷:99.59%(RSD=0.50%),牡荆素鼠李糖苷:99.57%(RSD=0.96%),牡荆素:98.70%(RSD=1.10%),芦丁:99.35%(RSD=1.16%),金丝桃苷:99.28%(RSD=0.88%)。结论:该方法准确可靠,重现性好,可用于山楂叶的质量控制。
文摘This paper reports that in the presence of cetyltrimethyl ammonium bromide as phase transfer catalyst,D-glucosamine hydrochloride reacts with 2,4-dinitrophenol to synthesize 1-O-(2’,4’-dinitrophenyl)-2-acetamido-β-D-glucoside.Chemical structure of the new compound was confirmed by elemental analysis,IR and UV.
文摘Four pyridazinone gluosodes 4 were synthesized by Koenig′s Knorr reaction of 6 (4 halophenyl) 3( 2H ) pyridazinone silver salt 2 with bromoacetylglucose 3.Treatment of 4 with dry ammonia at 0～-5℃ effected a removal of the acetyl protecting groups to yield compounds 5.When the substituent on the benaene ring was F or Cl ,O glucoside was synthesized principally.However,when the substituent was Br or I ,N glucoside was mainly obtained.Their structures were confirmed by 1H NMR,IR and elemental analysis.
文摘为克服目前合成方法存在收率较低,反应时间长、产品分离困难等不足,本文以β-D-葡萄糖、乙酰溴为原料,经乙酰化、溴代反应合成了糖基体2,3,4,6-O-四乙酰基-α-D-溴代葡萄糖,再与4-羟基苯甲醛衍生物经糖苷化反应合成了5种4-甲酰基苯基(2,3,4,6-O-四乙酰基)-β-D-葡萄糖苷衍生物。在合成4-甲酰基苯基(2,3,4,6-O-四乙酰基)-β-D-葡萄糖苷衍生物的过程中,采用10%(质量分数) Na OH溶液为缚酸剂,三(3,6-二氧杂庚基)胺(TDA-1)为相转移催化剂,反应物的收率为61%～69%,并应用核磁共振技术确定了产品的结构。该方法具有产品收率较高,反应温和、操作简单等优点。
文摘Starting from \%D\%\|galactose, per\|\%O\|\%acetylated (\%S\%)\|TBMB carboxylic acid derivant of methyl\|4\|amino\|4\|deoxy\|\%D\%\|glucopyranoside was prepared. The mechanism of the possible side reactions of the catalytic reduction from different types of azide sugar to the corresponding amino sugar was discussed. 1\|\%O\%\|Me\|protection was selected for preventing the intramolecular dehydration of the 4\|amino sugar, which was a key intermediate product in this synthetic process. The product was characterized by HRMS and \{\{\}\+1H NMR\} spectroscopy and will be used as a molecular model to develop a new identification method of the \%D, L\|\%configurations of amino sugar.
