Method and equipment for preparing cefotiam hydrochloride

Method and equipment for preparing cefotiam hydrochloride

CN
  • CN 101,648,961 A
  • Filed: 08/25/2009
  • Published: 02/17/2010
  • Est. Priority Date: 08/25/2009
  • Status: Active Grant
First Claim
Patent Images

1. method for preparing cefotiam chloride comprises:

  • (1) raw material A TC.HCl'"'"'s is syntheticRaw material A TA.HCl is fed intake in encloses container, behind the adding solvent, be cooled to-10~

    10 ℃

    , to wherein splashing into chlorizating agent, add catalyzer then, in-15~

    0 ℃

    of reaction 2~

    4h, reaction leaches the ATC.HCl crystallization after finishing;

    Wherein, the mass ratio of ATA.HCl and solvent is 1;

    5~

    8;

    The mol ratio of ATA.HCl and chlorizating agent is 1;

    1~

    3;

    The mol ratio of ATA.HCl and catalyzer is 1;

    1~

    2;

    (2) raw material 7-ACMT'"'"'s is synthetic7-ACA and DMMT 1;

    1 in molar ratio~

    1.5 are mixed in the solvent, add boron trifluoride complex, in 0~

    65 ℃

    of reaction 1~

    2h, reaction finishes the back cooling and adds the water hydrolysis for 20~

    25 ℃

    , adds antioxidant, drip alkali then and regulate pH to 2.5~

    3.0, lower the temperature 10~

    15 ℃

    , stir growing the grain 2~

    3h, filter, washing obtains the 7-ACMT fluoroborate;

    Wherein, the mass ratio of 7-ACA and solvent is 1;

    1.5~

    2.5;

    The mass ratio 3~

    5;

    1 of boron trifluoride complex and 7-ACA;

    The mass ratio of 7-ACA and antioxidant is 45~

    70;

    1;

    (3) cefotiam chloride is syntheticAbove-mentioned 7-ACMT is added alkali be dissolved in the water-containing solvent, add ATC.HCl and carry out acylation reaction, in-30~

    -10 ℃

    of reaction 1~

    2h, reaction is told organic phase after finishing, and adds concentrated hydrochloric acid at aqueous phase, adds hydrophilic solvent, separates out the cefotiam chloride crystallization;

    Wherein, 7-ACMT and alkali mass ratio be 1.5~

    4;

    1;

    The mass ratio of alkali and water-containing solvent is 1;

    10~

    15;

    The mass ratio of 7-ACMT and ATC.HCl is 1;

    0.6~

    1.5.

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