Cephalosporin antibiotic derivant
A compound and hydrate technology, applied in the field of medicine, can solve the problem of low sensitivity
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Embodiment 1
[0122] The preparation of embodiment 1 heterocycle
[0123] 1, the preparation of 2-(3-mercapto-azetidin-1-yl)-4,5-dihydroazole
[0124] In the reaction flask, add 35.2g (0.3mol) of 3-formylmercapto-azetidine and 500ml tetrahydrofuran, stir to dissolve, add 40g of powdery potassium carbonate, heat up to reflux, drop 2-bromo-4, 58.1g (0.35mol) / 200ml of 5-dihydrothiazole in tetrahydrofuran solution, after the dropwise addition, keep stirring and react for 2h, filter the reaction solution, concentrate to dryness under reduced pressure, add 200ml of 4mol / L hydrochloric acid, stir at room temperature for 2h, Adjust the pH above 8 with a dilute alkali solution, and a yellow solid precipitates out. The solid is purified with a methanol / acetone mixed solution, and the light yellow solid is 42.4 g, with a yield of 81%.
[0125] 2. Preparation of N-3-methyl-2-(3-mercapto-azetidin-1-yl)-4,5-dihydrothiazole chloride
[0126] In the reaction flask, add 35.2g (0.3mol) of 3-formylmercapt...
Embodiment 2
[0129] The preparation of embodiment 2 intermediate
[0130] 1. (6R,7R)-7-phenylacetamido-3-[[N-1-(4,5-dihydrothiazol-2-yl)-azetidin-3-yl]thio] Preparation of 8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid diphenylmethyl ester
[0131] In a dry reaction flask, (6R,7R)-7-phenylacetamido-3-hydroxy-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene- 50g (0.1mol) of diphenylmethyl 2-formate was dissolved in 300ml of dry acetone, 20ml of diisopropylethylamine was added dropwise at -15°C, and then 9ml of methanesulfonyl chloride was slowly added dropwise. Stir the reaction at ℃ for 1 h. After the reaction is completed, pour the reaction liquid into water, collect the precipitate, wash it with water, dry it fully, and put it into the next step directly.
[0132] Put 17.4 g (0.1 mol) of 2-(3-mercapto-azetidin-1-yl)-4,5-dihydrothiazole into a dry reaction flask, then add 200 ml of tetrahydrofuran solution, and then add powder Sodium carbonate 20g, add (6R, 7R)-7-phenylacetamid...
Embodiment 3
[0149] The preparation of embodiment 3 compounds of the present invention
[0150] 1. (6R,7R)-7-[[2-(5-Amino-1,2,4-thiadiazol-3-yl)-Z-2-methoximino]acetamido]-3- [[N-1-(4,5-dihydrothiazol-2-yl)-azetidin-3-yl]thio]-8-oxo-5-thia-1-azabicyclo [4.2.0] Preparation of oct-2-ene-2-carboxylic acid (i.e. compound 1-1)
[0151] Add (6R,7R)-7-amino-3-[[N-1-(4,5-dihydrothiazol-2-yl)-azetidin-3-yl]sulfanyl to a dry reaction flask ]-8-Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid diphenylmethyl ester is 18.1g (25mmol), anisole 40ml, in stirring , add 80ml of trifluoroacetic acid under cooling in an ice bath, stir at 10-15°C for 1.5h, after the reaction is complete, pour the reaction solution into 500ml of petroleum ether, filter, dissolve the filter cake in 200ml of absolute ethanol, wash with saturated sodium bicarbonate The solution was adjusted to pH 5-6, filtered, and the filter cake was washed twice with a small amount of acetone to obtain (6R, 7R)-7-[[2-(5-amino-1,2,4...
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