以5,6-二甲氧基-2-(4-吡啶基)-亚甲基-1-茚酮(Ⅱ)和溴化苄(Ⅲ)为原料,合成盐酸多奈哌齐的关键中间体1-苄基-4-(5,6-二甲氧基-1-茚酮-2-亚甲基)-吡啶(Ⅰ).研究了主要因素对反应的影响,n(Ⅱ)∶n(Ⅲ)=1∶1.3,反应时间60 m in,收率为92.8%....以5,6-二甲氧基-2-(4-吡啶基)-亚甲基-1-茚酮(Ⅱ)和溴化苄(Ⅲ)为原料,合成盐酸多奈哌齐的关键中间体1-苄基-4-(5,6-二甲氧基-1-茚酮-2-亚甲基)-吡啶(Ⅰ).研究了主要因素对反应的影响,n(Ⅱ)∶n(Ⅲ)=1∶1.3,反应时间60 m in,收率为92.8%.经核磁共振谱图分析确认为目标产物.进一步讨论了反应的动力学过程,并建立了动力学方程.展开更多
The synthesis process of 2-mercapto-5-methoxyimidazo[4,5-b]pyridine, a crucial intermediate of tenatoprazole which is a new proton pump inhibitor, was studied.2,6-Dichloropyridine as raw material was nitrated by nitri...The synthesis process of 2-mercapto-5-methoxyimidazo[4,5-b]pyridine, a crucial intermediate of tenatoprazole which is a new proton pump inhibitor, was studied.2,6-Dichloropyridine as raw material was nitrated by nitric acid/sulfuric acid, and after amination 2-amino-3-nitro-6-chloropyridine was obtained.It then reacted with sodium methoxide to give 2-amino-3-nitro-6-methoxypyridine and the intermediate was reduced by H2 with Raney Ni as catalyst to give 2,3-diamino-6-methoxypyridine.Finally cyclization was finished with carbon bisulfide to give the title compound.The optimal reaction conditions and yield(temperature, time, molar yield) were as follows: nitration,110℃, 8 h, 79.3%; amination, room temperature, 10 h, 87.6%; methoxylation,65℃, 30min, 98.7%; reduction,70℃, 3 h; cyclization, reflux, 4 h, 72.4% (two steps).The melting point of the title compound was the same as that reported in literature, and its structure was confirmed by 1H NMR.展开更多
文摘以5,6-二甲氧基-2-(4-吡啶基)-亚甲基-1-茚酮(Ⅱ)和溴化苄(Ⅲ)为原料,合成盐酸多奈哌齐的关键中间体1-苄基-4-(5,6-二甲氧基-1-茚酮-2-亚甲基)-吡啶(Ⅰ).研究了主要因素对反应的影响,n(Ⅱ)∶n(Ⅲ)=1∶1.3,反应时间60 m in,收率为92.8%.经核磁共振谱图分析确认为目标产物.进一步讨论了反应的动力学过程,并建立了动力学方程.
文摘The synthesis process of 2-mercapto-5-methoxyimidazo[4,5-b]pyridine, a crucial intermediate of tenatoprazole which is a new proton pump inhibitor, was studied.2,6-Dichloropyridine as raw material was nitrated by nitric acid/sulfuric acid, and after amination 2-amino-3-nitro-6-chloropyridine was obtained.It then reacted with sodium methoxide to give 2-amino-3-nitro-6-methoxypyridine and the intermediate was reduced by H2 with Raney Ni as catalyst to give 2,3-diamino-6-methoxypyridine.Finally cyclization was finished with carbon bisulfide to give the title compound.The optimal reaction conditions and yield(temperature, time, molar yield) were as follows: nitration,110℃, 8 h, 79.3%; amination, room temperature, 10 h, 87.6%; methoxylation,65℃, 30min, 98.7%; reduction,70℃, 3 h; cyclization, reflux, 4 h, 72.4% (two steps).The melting point of the title compound was the same as that reported in literature, and its structure was confirmed by 1H NMR.
文摘以鸡腿蘑发酵液中分离获得的具有抑制蛋白质非酶糖基化活性的新物质4,5-二羟基-2-甲氧基苯甲醛为对象,建立检测鸡腿蘑发酵液中该物质的高效液相色谱方法.其回归方程为Y=675.42X-943.39(r2=0.999 0),线性范围为1.23～123 mg/L.该方法的日内和日间精度分别为1.5%～5.6%,2.5%～4.6%,回收率为93.8%～96.6%.该方法能够在20 m in内完成一次分析,具有快速、准确、可靠的特点.
