2-脱氧链霉胺取代衍生物的结构确证和1H核磁定量

对新型氨基糖苷类抗生素合成中(本文阐述的是阿米卡星合成中的2个中间体，而非新型氨基糖苷类抗生素)的两个重要中间体进行结构确证和核磁定量。采用13C NMR、1H NMR、1H 1H-COSY、HMBC和MS对化合物1和化合物2进行了结构确证，并分别以马来酸和甲酸钠为内标物、D2O为溶剂，通过比较马来酸δ6.23ppm内标峰和化合物1δ5.05ppm、δ5.66ppm定量峰面积，以及甲酸钠δ8.36ppm内标峰和化合物2 δ2.00ppm、δ5.72ppm定量峰面积计算化合物1和化合物2的含量。化合物1为3-氨基-3-脱氧-α-D-葡吡喃糖基-(1→6)-2,3,4,6-四脱氧-2,6–二氨基-α-D-赤式-己吡喃糖基-(1→4)]-1-N-(2S)-4-氨基-2-羟基-1-氧丁基]-2-脱氧-D-链霉胺，化合物2为3-氨基-3-脱氧-α-D-葡吡喃糖基-(1→6)-2,3,4,6-四脱氧-2,6–二氨基-α-D-赤式-3-烯-己吡喃糖基-(1→4)]-1-N-(2S)-4-氨基-2-羟基-1-氧丁基]-2-脱氧-D-链霉胺，化合物1和化合物2的含量分别为64.98%和75.38%。化合物1和化合物2是2-脱氧链霉胺取代衍生物，采用氢核磁共振内标法可快速、准确地型氨基糖苷类抗生素合成过程中无商品化标准品的重要中间体进行定量分析。

Structure confirmation and determination of substituted 2-deoxystreptamines by proton nuclear magnetic resonance

The structures of two important intermediates in the synthesis of new kinds of aminoglycoside antibiotics were confirmed and the contents were determined by qNMR. The structures of the compound 1 and compound 2 were confirmed by 13C NMR, 1H NMR, 1H 1H-COSY, HMBC and MS. When maleic acid and sodium formate were respectively used as internal standards, and D2O was employed as solvent, the internal peak at δ6.23 for maleic acid and quantitative peaks at δ5.05 and δ5.66 for compound 1 and the internal peak at δ8.56 for sodium formate and quantitative peaks at δ2.00 and δ5.72 for compound 2 were obtained. The contents of compound 1 and compound 2 were calculated by comparing the response signal area of the sample and the internal standard. The compound 1 was 3-amino-3-deoxy-α-D-glucopyranosyl-(1→6)-2,3,4,6-tetradeoxy-2,6-diamino]-α-D-erythro-hexopyranosyl-(1→4)]-1-N-(2S)-4-amino-2-hydroxybutanoyl]-2-deoxy-D-streptamine and compound 2 was 3-amino-3-deoxy-α-D-glucopyranosyl-(1→6)-2,3,4,6-tetradeoxy-2,6-diamino]-α-D-erythro-hex-3-enopyranosyl-(1→4)]-1-N-(2S)-4-amino-2-hydroxybutanoyl]-2-deoxy-D-streptamine.The contents of compound 1 and compound 2 were 64.98% and 75.38%, respectively. The two compounds were substituted 2-deoxystreptamines and the keyintermediates, which standards couldn't be purchased, in the synthesis of new kinds of aminoglycoside antibiotics could be determined by qNMR rapidly and