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报道了用硫代硫酸钠脱去侧链保护氨基酸铜络合物中铜离子的新方法,该方法适用于合成Nδ-苄氧羰基鸟氨酸、Nδ-叔丁氧羰基鸟氨酸、Nδ-芴甲氧羰基鸟氨酸、Nδ-乙酰基鸟氨酸、Nδ-邻苯二甲酰基鸟氨酸、Nε-苄氧羰基赖氨酸、Nε-叔丁氧羰基赖氨酸、Nε-芴甲氧羰基赖氨酸、Nε-乙酰基赖氨酸、Nε-邻苯二甲酰基赖氨酸、γ-苄基谷氨酸、β-苄基天门冬氨酸.产物用元素分析法与1H NMR法进行了表征.探讨了反应温度、时间、投料比例、溶剂对脱铜反应的影响.实验结果表明,以硫代硫酸钠作为脱铜试剂,侧链保护氨基酸铜络合物与硫代硫酸钠的物质的量比为1∶1或1∶2,60℃反应1.5～2.0 h,收率与产物纯度均较高.该方法简便、高效、环境友好.
Reported the use of sodium thiosulfate to remove the side chain of copper amino acid copper complexes to protect the new method for the synthesis of Nδ-benzyloxycarbonyl ornithine, Nδ-tert-butoxycarbonyl ornithine, Nδ- Flunylmethoxycarbonylornithine, Nδ-acetylornithine, Nδ-phthaloylornithine, Nε-benzyloxycarbonyllysine, Nε-tert-butoxycarbonyllysine, Nε-fluorene N-acetyl lysine, Nε-phthalyl lysine, γ-benzyl glutamic acid, β-benzyl aspartic acid The product was characterized by elemental analysis with 1 H NMR The effects of reaction temperature, time, feed ratio and solvent on the copper removal reaction were discussed.The experimental results showed that using sodium thiosulfate as the copper removal reagent, the side chain protected amino acid copper complex and sodium thiosulfate Of the material ratio of 1: 1 or 1: 2, 60 ° C for 1.5 ~ 2.0 h, the yield and product purity are high. The method is simple, efficient and environmentally friendly.