（S）-2-aminobutyric acid being initial raw material,（S）-2-hydroxybutyric acid methyl ester was synthesized by means of a three step reaction of hydroxylation, salification and esterification. The product had a yiel...（S）-2-aminobutyric acid being initial raw material,（S）-2-hydroxybutyric acid methyl ester was synthesized by means of a three step reaction of hydroxylation, salification and esterification. The product had a yield rate of 60.4%, purity of 99% and ee value higher than 99% by characterization of GC, HPLC and 1H NMR. This synthesis technique has advantages of high purity and ee value, low cost, short reaction time and mild reaction conditions so that it is suitable for production on industrial scale.展开更多
3-Amino-2-methoxycarbonylthiophene used as the main raw material,an intermediate（thiofuran siamese） 2,4-dichloro-thieno[3,2-d]pyrimidine was synthesized.The prod-uct was characterized by nuclear magnetic resonance（...3-Amino-2-methoxycarbonylthiophene used as the main raw material,an intermediate（thiofuran siamese） 2,4-dichloro-thieno[3,2-d]pyrimidine was synthesized.The prod-uct was characterized by nuclear magnetic resonance（NMR）.The first step yield was 84%（190 ℃） and the second step yield was 81.4%（105 ℃,m（intermediate）：m（phosphorus oxychloride） = 1：6.4）.The raw product was refined with a unique refining process,which can enhance the purity up to 99.5% to meet the requirement of condi-tions for the development and research of thiofuran siamese as a new medicine of anticarcinogen.Contrasted with the traditional technique,this process featured with cheap raw materials,possible for solvent recovery and reuse,low comprehensive cost,and suit-able for production on certain scale.展开更多
文摘（S）-2-aminobutyric acid being initial raw material,（S）-2-hydroxybutyric acid methyl ester was synthesized by means of a three step reaction of hydroxylation, salification and esterification. The product had a yield rate of 60.4%, purity of 99% and ee value higher than 99% by characterization of GC, HPLC and 1H NMR. This synthesis technique has advantages of high purity and ee value, low cost, short reaction time and mild reaction conditions so that it is suitable for production on industrial scale.
基金Supported by the Innovation Fund for Technology Based Firms (10C26224212340)
文摘3-Amino-2-methoxycarbonylthiophene used as the main raw material,an intermediate（thiofuran siamese） 2,4-dichloro-thieno[3,2-d]pyrimidine was synthesized.The prod-uct was characterized by nuclear magnetic resonance（NMR）.The first step yield was 84%（190 ℃） and the second step yield was 81.4%（105 ℃,m（intermediate）：m（phosphorus oxychloride） = 1：6.4）.The raw product was refined with a unique refining process,which can enhance the purity up to 99.5% to meet the requirement of condi-tions for the development and research of thiofuran siamese as a new medicine of anticarcinogen.Contrasted with the traditional technique,this process featured with cheap raw materials,possible for solvent recovery and reuse,low comprehensive cost,and suit-able for production on certain scale.
