硼氢化还原法合成二氢高红霉素硼酸酯反应条件的优化

The Optimization of Hydride Boron Reaction Conditions in Dihydro High-Erythromycin Synthesis

以红霉素亚胺醚为原料,采用硼氢化物的催化还原体系合成二氢高红霉素硼酸酯,以TLC监测反应进程,探索了反应的适宜条件,并对样品进行了表征.结果表明:以甲醇-水为反应溶剂,Pt/C(w(Pt)=1.5%)为催化剂,在红霉素亚胺醚与硼氢化钾的物质的量之比为1:7、反应温度为5℃和反应时间为6 h等条件下,二氢高红霉素硼酸酯的产率高于95%,样品符合《中国药典》和《美国药典》中二氢高红霉素硼酸酯的质量要求.

The high-dihydro erythromycin borate was synthesized from erythromycin iminoether by using cata- lytic-reduction of boron hydride, and the progress was monitoring by TCL. The reaction conditions of optimization were researched and the product was characterized. The results showed that the suitable reaction conditions were methanol-water as solvent, Pt/C（w（Pt）=1.5%） as a catalyst, molar ratio of erythromycin iminoether and potassium borohydride 1 ： 7, reaction temperature 5 ℃, reaction time 6 h, and the yield was above 95%. The product is ac- cording with the quality standard of Chinese Pharmacopoeia and the United States Pharmacopoeia.