对羟基苯甘氨酸母液中一种杂质的分离与结构确证

Identification and Characterization of an Impurity in the Mother Liquor of p-Hydroxyphenylglycine

经萃取、解离、析晶、过滤等操作,提取对羟基苯甘氨酸母液中的一种杂质双(4-羟基苯基)乙酸。考察了萃取剂及萃取条件、析晶时间等参数对杂质提取效果的影响。优化条件下,杂质纯度达99.1%(HPLC)。杂质结构经MS、^(1)HNMR、^(13)CNMR、2DNMR等表征确证。

An impurity in the mother liquor of p-hydroxyphenylglycine was prepared by extraction,dissociation,crystallization and filtration.The effects of the extraction agent,extraction conditions and crystallization time on the extraction results were investigated,and the optimal extraction process was determined.The HPLC purity of the product was 99.1%(HPLC).The impurity was identified as bis(4-hydroxyphenyl)acetic acid by MS,^(1)H NMR,^(13)C NMR and 2D NMR.