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A technology of cefoxitin and compounds, applied in the field of pharmaceutical chemical synthesis, can solve the problems of insufficient product quality and yield competitiveness, raw materials or process conditions are not suitable for scale-up production, etc., to achieve easy control of product quality, avoid condensation side reactions, The effect of high production safety
Active Publication Date: 2016-07-06
山东安弘制药有限公司
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Problems solved by technology
[0014] The existing reported literatures all have the problem that the raw materials or process conditions are not suitable for scale-up production, or the product quality and yield are not competitive enough
Method used
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preparation example Construction
[0052] The preparation method of tert-butyl hypochlorite is synthesized with reference to the synthetic method in "Synthesis and Characterization of New Rubber Chlorinating Agent" (Li Yanli, Shi Shuxian, etc., Journal of Beijing University of Chemical Technology, 31(4):45~49);
[0053] N,N'-dibenzylethylenediamine diacetate was purchased from Shanghai Sinopharm Group Reagent Company, chlorosulfonyl isocyanate was purchased from Shanghai Bangcheng Chemical Company, and methanesulfonic acid was purchased from Shanghai Sinopharm Group Reagent Company.
Embodiment 1
[0055] A preparation method of cefoxitin, comprising the steps of:
[0056] (1) Add 200ml of dichloromethane (organic solvent A) to 1000ml of an aqueous solution of the compound of formula (IV) (containing 110g of deacetylcefalotin sodium), and then add 56g of N,N'-dibenzyl at a temperature of 30°C A solution made of ethylenediamine diacetate and 800ml of water, the compound of the intermediate formula (Ⅲ) structure was precipitated, cooled to 0-10°C and stirred for 2 hours; the precipitate was collected by filtration, washed with water and dichloromethane successively, vacuum Dry to obtain 132g of the intermediate compound of formula (III), with a yield of 95.2%;
[0057] through 1 HNMR (400MHz, CDCl 3 ) detection, the results are as follows:
[0066] The preparation method of cefoxitin as described in embodiment 1, difference is:
[0067] The organic solvent A described in the step (1) is chloroform, and 128.5 g of the compound of the intermediate formula (III) is obtained with a yield of 94.9%.
[0068] The compound of intermediate formula (Ⅲ) structure undergoes 1 HNMR (400MHz, CDCl 3 ) detection, the result is the same as in Example 1.
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Abstract
The invention relates to a method for preparing cefoxitin. The method includes that an organic solvent A is added into a compound aqueous solution in a formula (IV) structure, N, N'-dibenzyl ethylenediamine diacetate or N, N'-dibenzyl ethylenediamine diacetate aqueous solution is added, and filtering is performed to obtain an intermediate compound in a formula (III) structure; the intermediate compound in the formula (III) structure is added into acetone or tetrahydrofuran, chloriosulfonyl isocyanate is added for reaction, and hydrolyzing is performed after the reaction is finished; then ethyl acetate is added, salting-out is performed after filtering, extraction and decoloration, and filtering is performed to obtain an intermediate compound in a formula (II) structure; the intermediate compound in the formula (II) structure is added into an organic solvent B, organic acid is added for dissolution, a methanol solution of sodium methylate and hypochlorous acid tert-butyl ester are added for methyl oxidizing reaction, after the reaction is finished, sodium pyrosulfite and acetic acid are added for neutralization, water is added for extraction, and an aqueous phase is subjected to acid-out and filtering to obtain the cefoxitin. According to the method for preparing the cefoxitin, deacetyl cephalothin always exists in a mode of sodium salt or amine salt, condensation side reaction which is prone to occur due to low potential of hydrogen (pH) can be avoided, and product qualities and yield can be well controlled.
Description
[0001] This case is a divisional application of the patent application with application number 201210122034.9 technical field [0002] The invention relates to a preparation method of a compound, in particular to a preparation method of cefoxitin, and belongs to the technical field of pharmaceutical chemical synthesis. Background technique [0003] Cefoxitin Sodium, chemical name: (6R,7S)-3-carbamoyloxymethyl-7α-methoxy-8-oxo-7β-[2-(2-thienyl)B Amino]-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate sodium is a semi-synthetic cephamycin antibiotic developed by Merck Company of the United States and belongs to the second generation Cephalosporin antibiotics. Cefoxitin sodium has a strong antibacterial effect on Gram-negative bacteria, and its antibacterial spectrum includes Escherichia coli, Klebsiella pneumoniae, indole-positive Proteus and Serratia, Klebsiella, influenza bacillus, Salmonella, and Shigella Wait. It also has a good effect on staphylococcus and various str...
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