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以盐酸羟胺、三乙胺和丁二酸酐为原料,以1,4-二氧六环和少量的水为溶剂,EDTA三钠盐为稳定剂,以1-羟基苯并三氮唑(HOBT)为催化剂,一步反应制得标题化合物。当n(盐酸羟胺)∶n(丁二酸酐)∶n(EDTA三钠盐)∶n(1-羟基苯并三氮唑)=1.01∶1∶0.000 3∶0.01,溶剂V(二氧六环)∶V(水)=20∶1,中和反应温度为20℃,后续反应温度为120℃,反应时间为6 h时,高真空除水,反应收率达87.5%,产品纯度≥99.6%。
Using hydroxylamine hydrochloride, triethylamine and succinic anhydride as raw materials, 1,4-dioxane and a small amount of water as solvent, EDTA trisodium salt as stabilizer, 1-hydroxybenzotriazole (HOBT) As catalyst, one step reaction to give the title compound. When n (hydroxylamine hydrochloride): n (succinic anhydride): n (trisodium EDTA): n (1-hydroxybenzotriazole) = 1.01:1:0.000 3:0.01, the solvent V ): V (water) = 20: 1, the neutralization reaction temperature is 20 ℃, the subsequent reaction temperature is 120 ℃, the reaction time is 6 h, the high vacuum dewatering, the reaction yield of 87.5%, product purity ≥ 99.6% .