Preparation method of cephalosporin dimer compound
A technology for compounds and cephalosporins, applied in the field of preparation of cephalosporins dimers, can solve the problems of low purification of cephalosporins dimers, difficulty in purifying target products, difficulty in purification process, etc., and achieves practical value and social and economic benefits. , The effect of eliminating potential safety hazards and easy operation
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0025] Example 1: Preparation of cefditoren pivoxil dimer compound
[0026] 1) Preparation of Vilsmeier reagent
[0027] 0.24g (0.8mmol) of bis-(trichloromethyl)carbonate was added in batches to the reaction solution of 50ml N,N-dimethylformamide at 0°C, and the temperature was controlled to 5°C to prepare 2.4mmol of Vilsmeier reagent;
[0028] 2) Preparation of dimer compounds
[0029] The Vilsmeier reagent in step 1 was stirred for 30 min, 1.24 g (2.0 mmol) of cefditoren pivoxil was added, and the temperature was controlled at 0 °C to react for 12 hours; then, 40 ml of dichloromethane and 100 ml of water were added to the reaction solution, and 2 The pH of the solution was adjusted to 6.0 with % sodium bicarbonate solution, and the solution was separated. The organic phase was washed successively with 40 ml of 2% sodium bicarbonate solution, 100 ml of saturated brine, and 100 ml of water. The organic phase was concentrated under reduced pressure, purified by column chromato...
Embodiment 2
[0030] Example 2: Preparation of cefpodoxime axetil dimer compound
[0031] 1) Preparation of Vilsmeier reagent
[0032] 0.36g (1.2mmol) of bis-(trichloromethyl)carbonate was added in batches to the reaction solution of 0.27g (3.6mmol) of N,N-dimethylformamide and 50ml of dichloromethane at 0°C, and the temperature was controlled. At 5°C, prepare 3.6 mmol of Vilsmeier reagent;
[0033] 2) Preparation of dimer compounds
[0034] The Vilsmeier reagent in step 1 was stirred for 30 min, 0.56 g (1 mmol) of the crude drug cefpodoxime axetil was added, and the temperature was controlled at 15° C. to react for 5 hours. Then, 40 ml of chloroform and 100 ml of water were added to the reaction solution, the pH of the solution was adjusted to 7.0 with 6% sodium bicarbonate solution, and the layers were separated. , the organic phase was concentrated under reduced pressure, purified by column chromatography, and the eluent was a mixed solvent of ethyl acetate: petroleum ether=10:1 to ob...
Embodiment 3
[0035] Example 3: Preparation of cefotaxime dimer compound
[0036] 1) Preparation of Vilsmeier reagent
[0037] 0.20g (0.67mmol) of bis-(trichloromethyl)carbonate was added in portions at 3°C with 0.16g (2.0mmol) of N,N-dimethylformamide and 50ml of 1,2-dichloroethane 2.0 mmol of Vilsmeier reagent was prepared in the liquid, and the temperature was controlled at 2 °C;
[0038] 2) Preparation of dimer compounds
[0039] The Vilsmeier reagent in step 1 was stirred for 30 min, 0.90 g (2.0 mmol) of cefotaxime crude drug was added, and the temperature was controlled at 35° C. to react for 2 hours. Then, 80ml of ethyl acetate and 100ml of water were added to the reaction solution, the pH of the solution was adjusted to 8.0 with 4% sodium bicarbonate solution, the layers were separated, and the organic phase was washed with 80ml of 2% sodium bicarbonate solution, 100ml of saturated brine, Wash with 100 ml of water, concentrate the organic phase under reduced pressure, and purif...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More