Synthesis of istradefylline / 军事医学

Objective To optimize the synthesis process of istradefylline 1 for industrial production.Methods Istrade-fylline was synthesized from dimethyl carbonate and ethylamine through a series reactions including condensation,cycliza-tion,nitrosation,and reduction to produce 1,3-diethyl-5,6-diaminouracil(6),which was subjected to amidation with (E)-3,4-dimethoxycinnamic acid (8),followed by cyclization and methylation reaction.Compound 8 was prepared from veratr-aldehyde and propanedioic acid by Knoevenagel condensation.The structures of intermediate and target compounds were confirmed by MS and 1 H-NMR.Results and Conclusion The quality control points of each key process were optimized so that the total yield was 26.2% and the purity of the product was 99.76%.This improved synthesis method has some advan-tages,such as mild reaction conditions,simple operation,and applicability to industrial production.

Synthesis of phacolysin / 军事医学

Objectve To optimize the synthesis process of phacolysin 1 for industrial production.Methods Phacolysin as the target product was synthesized with a total yield of 40.7% by condensation reaction of O-phenylenediamine and sulfonation reaction.The yield reported in literature was 24.8%.Results Such factors as the ratio of the raw materials,the catalyst,and the reaction time were inveatigated and optimized to make the reaction conditions mild and easy to control with less side effect.Conclusion The structure is confirmed by 1HNMR and MS,and the optimized process is more suitable for industrial production.