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.
