Preparation method of cefditoren pivoxil [delta]3 isomer
A technology of cefditoren pivoxil and cefditoren, which is applied in the field of pharmaceutical intermediate synthesis, can solve the problems of low isomerization conversion rate, difficult extraction, difficult selection of mobile phases, etc. Short time, solve the effect of poor selection of mobile phase
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Embodiment 1
[0042] In a clean reaction flask, 32.3g (0.1mol, 1eq) of cephalosporin nucleus 7-ATCA shown in formula II was dissolved in 323g of dichloromethane, and then 50.9g (0.25mol, 2.5eq) of BSA (N, O-bistrimethylsilylacetamide), after stirring evenly, add 11.1g (0.11mol, 1.1eq) organic base triethylamine at 25-35°C and control the temperature at 25-30°C for isomerization Reaction, stirring and reacting for 0.5 to 1 hour. After the isomerization reaction, control the temperature of the reaction liquid at 25 to 35°C, add 100 mL of water to the reaction liquid, stir for 5 to 15 minutes, and let it stand for sufficient stratification. Remove the organic layer, collect the water layer feed solution in the reaction bottle, and control the temperature at 25-35°C, add 5% dilute hydrochloric acid solution to the water layer feed solution, adjust the pH value to 2.0-3.0, adjust After it is basically stable, slowly lower the temperature to 5-15°C and carry out stirring and crystallization for 1...
Embodiment 2
[0046]In a clean reaction flask, 32.3 g (0.1 mol, 1 eq) of cephalosporin nucleus 7-ATCA shown in formula II was dissolved in 485 g of dichloromethane, and then 61 g (0.3 mol, 3.0 eq) of BSA (N, O -bistrimethylsilylacetamide), after stirring evenly, add 15.2g (0.15mol, 1.5eq) organic base triethylamine at 25-30°C and control the temperature to carry out isomerization reaction at 25-30°C , stirred and reacted for 1.0 hour. After the isomerization reaction was completed, 150 mL of water was added to the reaction solution at a temperature of 25 to 30 ° C, stirred for 15 minutes, and after standing for sufficient separation, the organic layer was separated and discarded. Collected The water layer feed liquid is in the reaction bottle, and the temperature is controlled at 25-35°C. Add a 10% mass percent dilute hydrochloric acid solution to the collected water layer feed liquid to adjust the pH value to 2.0-2.5, and adjust it to be basically stable. Afterwards, slowly lower the tempe...
Embodiment 3
[0050] In a clean reaction flask, 32.3 g (0.1 mol, 1 eq) of cephalosporin nucleus 7-ATCA shown in formula II was dissolved in 400 g of ethyl acetate, and then 40.7 g (0.2 mol, 2.0 eq) of BSA (N, O-bistrimethylsilylacetamide), after stirring evenly, add 20.2g (0.2mol, 2.0eq) diisopropylamine at 25-30°C and control the temperature at 25-30°C for isomerization Reaction, stirring and reacting for 1.0 hour, after the isomerization reaction, control the temperature of the reaction solution at 25-30°C, add 150mL of water to the reaction solution, stir for 15 minutes, after standing for sufficient separation, separate the liquid and discard the organic layer, Collect the water layer feed liquid in the reaction bottle, and control the temperature at 25-35°C, add 10% dilute hydrochloric acid solution to the collected water layer feed liquid, adjust the pH value to 2.5-3.0, and adjust the basic After stabilization, slowly lower the temperature to 5-10°C and fully stir and crystallize for...
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