3-[α-甲氧基亚氨基-α-(2-羟基苯基)-甲基]-5,6-二氢-1,4,2-二噁嗪的合成

Synthesis of(5,6-Dihydro-1,4,2-dioxazin-3-yl)(2-hydroxyphenyl)methanone O-Methyl Oxime

[目的]3-[α-甲氧基亚氨基-α-(2-羟基苯基)-甲基]-5,6-二氢-1,4,2-二噁嗪是甲氧基丙烯酸酯类杀菌剂的一个重要中间体。[方法]以邻羟基苯乙酸甲酯为原料,经羟基保护、肟化、甲基化、环合、脱保护合成3-[α-甲氧基亚氨基-α-(2-羟基苯基)-甲基]-5,6-二氢-1,4,2-二噁嗪。[结果]在优化的反应条件下,反应总收率为27.0%(以邻羟基苯乙酸甲酯计),含量为98.5%,其结构经1H NMR和红外分析确认。[结论]该工艺简单经济,条件温和,适合工业化生产。

（5,6-Dihydro-1,4,2-dioxazin-3-yl）（2-hydroxyphenyl）methanone O-methyl oxime is an important intermediate of methoxy-acrylate fungicides.[Methods]（5,6-Dihydro-1,4,2-dioxazin-3-yl）（2-hydroxyphenyl）methanone O-methyl oxime can be obtained through hydroxyl protection,oxime,methylation,cyclization and deprotection reactions using methyl 2-（2-hydroxyphenyl）acetate as starting material.[Results] The total yield was 27.0% based on methyl 2-（2-hydroxyphenyl）acetate under the optimized reaction conditions and purity was as high as 98.5%.The structure of the end product was confirmed by 1H NMR and IR.[Conclusions] This process is simple,warm and economical,which make it very suitable for industrial production.