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目的:确定合成氟氧头孢关键中间体表-噁唑啉并氮杂环丁酮(A)及其对映异构体噁唑啉并氮杂环丁酮(G)的反应条件。方法:A和G按文献方法分别以6α-苯甲酰基青霉素烷酸二苯甲酯亚砜和6β-苯甲酰基青霉素烷酸二苯甲酯亚砜为原料,三苯基膦为脱硫试剂合成;以收率为指标,确定较佳的反应温度、时间等反应条件。结果:制备得到了化合物A(收率78%,纯度98.1%)和G(收率80%)并经结构表征证实。A的反应条件为:不加酸性催化剂,在80～90℃下反应10h;G的反应条件为:加入酸性催化剂。2种化合物的合成中均应除去生成的水分以使收率提高。结论:以确定的反应条件可得到目标化合物,且适合工业化生产。
OBJECTIVE: To determine the reaction conditions for the synthesis of the key intermediates for the synthesis of fluoxetine and its enantiomers, oxazoline and azetidinone (G). Methods: A and G were prepared by literature method using 6α-benzoylpenicillin alkylate diphenylmethyl sulfoxide and 6β-benzoylpenicillin alkanoate diphenylmethyl sulfoxide as raw materials, and triphenylphosphine as the desulfurization reagent ; The yield as an indicator to determine the better reaction temperature, time and other reaction conditions. Results: Compound A (78% yield, 98.1% purity) and G (80% yield) were prepared and confirmed by structural characterization. The reaction conditions of A are: without acidic catalyst, the reaction at 80 ~ 90 ℃ for 10h; G reaction conditions: adding an acidic catalyst. In the synthesis of both compounds, the generated water should be removed to increase the yield. Conclusion: The target compound can be obtained under certain reaction conditions and is suitable for industrial production.