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    • 4. 发明授权
    • Preparation method of high-purity L-carnitine
    • 高纯度左旋肉碱的制备方法
    • US09096493B2
    • 2015-08-04
    • US13121392
    • 2009-10-09
    • Shuhua GuXuecheng WangQingyi Li
    • Shuhua GuXuecheng WangQingyi Li
    • C07C229/22
    • C07C229/22C07B2200/07
    • The present invention relate to a preparation method of high-purity L-carnitine which belongs to an important technique of quality control in different steps of chiral medicine production. The method comprises the following steps of: monitoring the content of the L-isomer impurity in chiral material S-epichlorohydrin by gas chromatography and chiral column and controlling the content of the L-isomer impurity in chiral raw material in the definite range; monitoring and controlling the specific optical rotation of the chiral intermediate L-3-chloro-2-hydroxy-N,N,N-trimethyl-propanaminium in the definite ranges using a polarimeter; monitoring the content of the R-isomer in the intermediate L-3-cyano-2-hydroxy-N,N,N-trimethyl-propanaminium using derivation agent (+)α-methyl-6-methoxy-2-naphthaleneaceyl chloride by HPLC and controlling the content of the isomer in the intermediate in the definite range; and measuring the final product L-carnitine using derivation agent (+)α-methyl-6-methoxy-2-naphthaleneaceyl chloride by HPLC. This method gives the high-purity L-carnitine in which the content of L-isomer may be more than 97% and that of R-isomer less than 2%.
    • 本发明涉及高纯度L-肉碱的制备方法,属于手性药物生产不同步骤中质量控制的重要技术。 该方法包括以下步骤:通过气相色谱和手性柱监测手性物质S-表氯醇中L-异构体杂质的含量,控制手性原料中L-异构体杂质的含量在一定范围内; 使用偏光计监测和控制手性中间体L-3-氯-2-羟基-N,N,N-三甲基 - 丙胺在一定范围内的比旋光度; 使用衍生剂(+)α-甲基-6-甲氧基-2-萘甲酰氯通过HPLC监测中间体L-3-氰基-2-羟基-N,N,N-三甲基 - 丙胺中R-异构体的含量 并控制中间体中异构体的含量在一定范围内; 并使用衍生剂(+)α-甲基-6-甲氧基-2-萘甲酰氯通过HPLC测定最终产物L-肉毒碱。 该方法给出L-异构体含量高于97%,R-异构体含量低于2%的高纯度左旋肉碱。
    • 9. 发明申请
    • PREPARATION METHOD OF HIGH-PURITY L-CARNITINE
    • 高效L-CARNITIN的制备方法
    • US20110263897A1
    • 2011-10-27
    • US13121392
    • 2009-10-09
    • Shuhua GuXuecheng WangQingyi Li
    • Shuhua GuXuecheng WangQingyi Li
    • C07C227/12
    • C07C229/22C07B2200/07
    • The present invention relate to a preparation method of high-purity L-carnitine which belongs to an important technique of quality control in different steps of chiral medicine production. The method comprises the following steps of: monitoring the content of the L-isomer impurity in chiral material S-epichlorohydrin by gas chromatography and chiral column and controlling the content of the L-isomer impurity in chiral raw material in the definite range; monitoring and controlling the specific optical rotation of the chiral intermediate L-3-chloro-2-hydroxy-N,N,N-trimethyl-propanaminium in the definite ranges using a polarimeter; monitoring the content of the R-isomer in the intermediate L-3-cyano-2-hydroxy-N,N,N-trimethyl-propanaminium using derivation agent (+)α-methyl-6-methoxy-2-naphthaleneaceyl chloride by HPLC and controlling the content of the isomer in the intermediate in the definite range; and measuring the final product L-carnitine using derviation agent (+)α-methyl-6-methoxy-2-naphthaleneaceyl chloride by HPLC. This method gives the high-purity L-carnitine in which the content of L-isomer may be more than 97% and that of R-isomerless than 2%.
    • 本发明涉及高纯度L-肉碱的制备方法,属于手性药物生产不同步骤中质量控制的重要技术。 该方法包括以下步骤:通过气相色谱和手性柱监测手性物质S-表氯醇中L-异构体杂质的含量,控制手性原料中L-异构体杂质含量在一定范围内; 使用偏光计监测和控制手性中间体L-3-氯-2-羟基-N,N,N-三甲基 - 丙胺在一定范围内的比旋光度; 使用衍生剂(+)α-甲基-6-甲氧基-2-萘甲酰氯通过HPLC监测中间体L-3-氰基-2-羟基-N,N,N-三甲基 - 丙胺中R-异构体的含量 并控制中间体中异构体的含量在一定范围内; 并用高效液相色谱法测定最终产物L-肉碱,使用脱甲剂(+)α-甲基-6-甲氧基-2-萘甲酰氯。 该方法得到L-异构体的含量高于97%的高纯度左旋肉碱,R异构体的含量高于2%。