摘要
3,4-二氨基吡啶与乙二醛环化得到吡啶并[3,4-b]吡嗪,进一步与氯甲酸乙酯在硼氢化锂的作用下发生还原反应得到乙基5,6-二氢吡啶并[3,4-b]吡嗪-6(5H)-羧酸酯,然后经钯碳氢化得到乙基-5,6,7,8-四氢-二氢吡啶并[3,4-b]吡嗪-6(5H)-羧酸酯,最后在碱性条件下去保护基团合成了5,6,7,8-四氢吡啶并[3,4-b]吡嗪。对还原反应进行了工艺研究,确定优化反应条件:硼氢化锂为还原剂,反应时间为1 h,反应温度为-15℃。总收率为48.4%。产品结构经1H NMR确证。
Pyrido [3,4-b]pyrazine（1）,which was synthesized from 3,4-diaminopyridine and gloxyal,was converted into ethyl-pyrido[3,4-b]pyrazine-6（5H）-carboxylate（2） in lithium borohydride catalyzed reduction process.2 was further transformed to the title compound（4） in several reaction steps.The preparation of 2 is critical to the whole process,therefore its reaction conditions were optimized.The target compound was achieved in overall yield of 48.4% and confirmed with 1H NMR.
出处
《精细化工中间体》
CAS
2010年第5期49-51,共3页
Fine Chemical Intermediates
