苯并呋喃-2,3-二酮3-（O-甲基-肟）2-肟合成工艺研究

Synthesis of 3-(methylimino)benzofuran-2(3H)-one oxime

摘要:

以4-羟基-3-硝基香豆素为起始原料，经过开环、脱羧，得到2-硝基-2，-羟基苯乙酮，再和甲氧胺盐酸盐反应生成中间体1-（2-羟基苯基）-2-硝基-乙酮-O-甲基肟。最后通过碱性条件下关环得到苯并呋喃-2,3-二酮3-（O-甲基-肟）2-肟。目标化合物及中间体结构经1H-NMR确证。反应总收率70.4%，产品纯度99.2%。该工艺原料廉价，操作简单，收率较高，具有较好的工业化应用前景。

Abstract:

1-(2-Hydroxyphenyl)-2-nitroethanone were synthesized through ring opening reaction of 4-Hydroxy-3-nitrocoumarin and the subsequent decarboxylation. Treating it with methoxyamine hydrochloride gave 1-(2-hydroxyphenyl)-2-nitroethanone O-methyl oxime, which underwent closing reaction mediated by sodium carbonate and gave 3-(methylimino)benzofuran-2(3H)-one oxime. Structures of all intermediates and target product were characterized by 1H NMR. The total yield was 70.4% and purity was as high as 99.2%. The synthetic process has features in high yield, easy operation, which are very promising in industrialization.