喹赛多的合成工艺研究

The Synthesis Technologic Study of Cyadox

关键词:  喹赛多  合成工艺研究  苯并呋咱-N-氧化物  Beirut反应

Key words:  cyadox  synthesis study  benzofuroxan-N-oxide  Beirut reaction  Hydrazoning reaction

摘要:

以苯并呋咱-N-氧化物和丙酮醛缩二甲醇为起始原料，N,N-二甲基甲酰胺为溶剂，吡咯烷为催化剂，经过Beirut反应得到喹噁啉-1,4-二氧-2-甲醛缩二甲醇，喹噁啉-1,4-二氧-2-甲醛缩二甲醇在以甲醇为溶剂、浓盐酸为催化剂的条件下与氰乙酰肼反应生成喹赛多。终产物喹赛多经核磁共振氢谱、核磁共振碳谱、质谱、红外光谱进行确证。总收率为55.8%。

Abstract:

2-formylquinoxaline-1, 4-dioxide dimethylacetal was obtained by benzofuroxan-N-oxide and pyruvaldehyde dimethylacetal which were dissolved in N,N-dimethyl formamide and pyrrolidine was used as catalyzer. 2-formylquinoxaline-1, 4-dioxide dimethylacetal was dissolved in methanol and concentrated hydrochloric acid, then reacted with cyanoacetylhydrazine to obtain cyadox. Cyadox was identified by ¹H-NMR, ^{13C-NMR, MS, and IR. The total yield was 55.8%.}