7-ATCA的环保合成新方法

Study on the Green Synthesis Methods 7-ATCA

改进了头孢母体3-(1-甲基-1-H-四氮唑-5-基)硫代甲基7-氨基头孢烷酸(7-ATCA)的合成工艺,水解后对溶媒进行萃取回收,在水相中进行结晶,减少了污染更加环保。对催化剂进行甄别后,采用BF_3·CH_3O-COOCH_3络合物替代传统的BF_3·CH_3CN络合物或BF_3·CH_3CH_2OCH_2CH_3络合物催化7-ACA和甲巯四氮唑合成头孢母体7-ATCA。确定了甲巯四氮唑与7-ACA合适的反应条件和检测反应终点的检测方法以及萃取剂的用量及萃取次数,产品收率≥115%,含量≥99%。

To improve the manufacturing process of cephalosporin nucleus 7-amino-3- （1-methyl-1-H-tetrazol-5- yhhiomethyl-3-eephem-4-carboxylicaeid （7 -ATCA）, solvent was extracted and recovered after hydrolysis, crystallized in water, to reduce the pollution and was more environmentally friendly. After the catalysts were compared, boron trifluoride acetonitrile complex or boron trifluoride ethyl ether complex, which were the traditional boron trifluoride complexes, were substituted by boron trifluoride dimethyl carbonate complex to catalyze the reaction of 7-ACA and 5- mercapto-1- methyhetrazole to prepare 7- ACT. Appropriate mole proportion of boron trifluoride dimethyl carbonate complex and 7-ACA was determined, reaction for the detection of endpoint detection method resulting product yield was exceeding 115% and assay was exceeding 99%.