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目的改进喜树碱全合成关键中间体的合成工艺。方法以叔丁醇钾代替金属氢化物 ,于THF中制备 6 氰基 1,1 亚乙二氧基 7 乙氧羰基甲基 5 氧代 Δ6(8) 四氢中氮茚 (6 ) ,并以 6于DMF和THF混和溶剂中在冰浴下制备 6 氰基 1,1 亚乙二氧基 7 (1′ 乙氧羰基 )丙基 5 氧代 Δ6(8) 四氢中氮茚 (2 )。结果和结论改进后的工艺降低了反应的危险性 ,并避免了 - 78℃的超低温 ,同时以价廉的溶剂代替较贵的溶剂 ,降低了成本 ,此外 ,制备过程中的两个中间体 (化合物 4、5 )不需纯化 ,简化了工艺。
Objective To improve the synthetic process of camptothecin, a key intermediate for total synthesis. Methods 6-Cyano-1,1-ethylenedioxy-7-ethoxycarbonylmethyl 5-oxo-6 (8) tetrahydroindolizine (6) was prepared in THF using potassium tert-butoxide instead of the metal hydride, 6 6 cyano 1, 1 ethylenedioxy 7 (1 ’ethoxycarbonyl) propyl 5 oxo [Delta] 6 (8) tetrahydroindolizine (2) was prepared in a DMF and THF mixed solvent under an ice bath. Results and Conclusions The improved process reduces the risk of reaction and avoids cryogenic temperatures of -78 ° C, while replacing the more expensive solvents with less expensive solvents, reducing costs. In addition, two intermediates ( Compounds 4, 5) do not require purification, simplifying the process.