摘要
目的优化2,5-二乙酰氧甲基-3,6-二甲基吡嗪的合成工艺。方法以川芎嗪为原料,在冰乙酸条件下经过30%H2O2氧化后,采用液态加料法与醋酐酯化反应得到目标产物;以高效液相色谱法,进行目标产物与对照品吸收峰峰面积的对比来计算产率,并考察反应温度和时间对酯化反应产率的影响。结果改进了合成工艺,简化了操作,总产率提高到69.12%。结论改进后的工艺切实可行,可操作性好,更适合工业化生产。
Objective To synthesize 2,5-diacetoxymethyl-3,6-dimethylpyrazine and to optimize technical conditions.Methods Tetramethylpyrazine and 30% hydrogen peroxide were reacted in glacial acetic acid to yield N,N-dioxotetramethylpyrazine,then heated and esterified to get target product.The yield was monitored by comparing peak area of target product with reference substance in HPLC.The reaction temperature and time were investigated by the method of liquid feeding.Results The synthetic process was improved,the operation was simplified and the overall yield was increased to 69.12%.Conclusion The improved synthetic process is practicable and suitable for large-scale manufacture
出处
《中国医药导报》
CAS
2012年第7期109-109,114,共2页
China Medical Herald
基金
国家自然科学基金资助项目(项目编号:81072542)
江苏省自然科学基金资助项目(项目编号:BK2011077)
