Method for preparing tebipenem ester
A technology of tebipenem and ethyl acetate, applied in the direction of organic chemistry and the like, can solve problems such as being unsuitable for industrialized production, taking a long time, etc., and achieving the effects of easy recovery, resource saving and simple operation
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Embodiment 1
[0030] React 1.37g of tipipenem, 11ml of N,N-dimethylformamide, 0.5g of potassium carbonate, and 0.03g of tetrabutylammonium bromide at -10°C for 0.5h, and add pipenem dropwise at this temperature Iodomethyl 0.88g, after the reaction was completed, 11ml of ethyl acetate was added to filter off the insoluble matter, the filtrate was washed with 22ml of water, the aqueous phase was extracted once with 11ml of ethyl acetate, the ethyl acetate was combined, washed with water, and the ethyl acetate was added with 11ml of water. Adjust the aqueous solution of citric acid to 3.5, separate the phases, wash the aqueous phase with 11ml of ethyl acetate, add 22ml of ethyl acetate to the aqueous phase, adjust to 7.5 with aqueous sodium bicarbonate, separate the phases, wash the ethyl acetate phase with 22ml of water, and add 22ml of ethyl acetate to the aqueous phase. Add 0.5 g of anhydrous sodium sulfate and activated carbon to dry and decolorize, concentrate the filtrate to a certain vol...
Embodiment 2
[0032] React 1.37g of tipipenem, 11ml of N,N-dimethylacetamide, 0.5g of potassium carbonate, and 0.03g of tetrabutylammonium bromide at -10°C for 0.5h, and add pipenem dropwise at this temperature Iodomethyl 0.88g, after the reaction was completed, 11ml of ethyl acetate was added to filter off the insoluble matter, the filtrate was washed with 22ml of water, the aqueous phase was extracted once with 11ml of ethyl acetate, the ethyl acetate was combined, washed with water, and the ethyl acetate was added with 11ml of water. Adjust the aqueous solution of citric acid to 3.5, separate the phases, wash the aqueous phase with 11ml of ethyl acetate, add 22ml of ethyl acetate to the aqueous phase, adjust to 7.5 with aqueous sodium bicarbonate, separate the phases, wash the ethyl acetate phase with 22ml of water, and add 22ml of ethyl acetate to the aqueous phase. Add 0.5 g of anhydrous sodium sulfate and activated carbon to dry and decolorize. The filtrate is concentrated to a certain...
Embodiment 3
[0034] React 1.37g tipipenem, 11ml N,N-dimethylacetamide, 0.6g potassium carbonate, and 0.03g tetrabutylammonium bromide at -20°C for 0.5h, then add pipenem dropwise at this temperature Iodomethyl 1.05g, after the reaction was completed, add 11ml of ethyl acetate to filter off the insoluble matter, wash the filtrate with 22ml of water, extract the water phase once with 11ml of ethyl acetate, combine the ethyl acetate, wash with water, add 11ml of water to the ethyl acetate, and use Adjust the aqueous solution of citric acid to 3.5, separate the phases, wash the aqueous phase with 11ml of ethyl acetate, add 22ml of ethyl acetate to the aqueous phase, adjust to 7.5 with aqueous sodium bicarbonate, separate the phases, wash the ethyl acetate phase with 22ml of water, and add 22ml of ethyl acetate to the aqueous phase. Add 0.5 g of anhydrous sodium sulfate and activated carbon to dry and decolorize. The filtrate is concentrated to a certain volume, stirred and crystallized, cooled ...
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