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在微波辐射条件下,以氯二氟乙酸钠为促进剂,实现2-羟基苯乙酮肟一锅法制备苯并异口恶唑反应。考察了不同促进剂及用量、溶剂、碱、温度以及微波功率对反应的影响。确定最优反应条件为:n(2-羟基苯乙酮肟)∶n(氯二氟乙酸钠)∶n(碳酸钾)=1.0∶1.5∶1.5,溶剂为N,N-二甲基乙酰胺(2-羟基苯乙酮肟的浓度为1 mol/L),微波功率为300 W,反应温度为85℃,反应时间为35 min。在最优条件下,以64%~93%的收率得到8种含不同取代基的苯并异口恶唑类化合物。用1HNMR和MS对目标产物的结构进行了表征。
Under the condition of microwave irradiation, sodium chlorodifluoroacetate was used as a promoter to produce 2-hydroxyacetophenone oxime in one-pot to prepare benzisoxazole. The effects of different promoters and their dosage, solvent, alkali, temperature and microwave power on the reaction were investigated. The optimum reaction conditions were as follows: n (2-hydroxyacetophenone oxime) :n (sodium chlorodifluoroacetate) :n (potassium carbonate) = 1.0:1.5:1.5 and the solvent was N, N-dimethylacetamide (2-hydroxyacetophenone oxime was 1 mol / L), the microwave power was 300 W, the reaction temperature was 85 ℃ and the reaction time was 35 min. Under the optimum conditions, eight kinds of benzo iso-isooxazole compounds with different substituents were obtained in 64% ~ 93% yield. The structure of the target product was characterized by 1H NMR and MS.