Derivant of cephalosporin of amidinothioacetamide, preparation method and application
A cephalosporin, cephalosporanic acid technology, applied in the direction of pharmaceutical formulations, antibacterial drugs, medical preparations containing active ingredients, etc.
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Embodiment 1
[0053] Preparation of intermediate 7-bromoacetamido-3-chloro-3-cephem-4-carboxylic acid
[0054] 2.34g7-amino-3-chloro-3-cephem-4-carboxylic acid (7-ACCA) was added to 30mlH 2 O, and then add 30ml of toluene. Stir in an ice-water bath, and when the temperature drops to 0-5°C, slowly add 1.4ml of triethylamine dropwise, and the 7-amino-3-chloro-3-cephem-4-carboxylic acid in the system is completely dissolved. Then add bromoacetyl bromide dropwise in batches, first add 0.8ml bromoacetyl bromide dropwise, stir rapidly, raise the temperature to 25-30°C, and add NaHCO dropwise at the same time 3 solution (5%) until the system is completely clear; after 20 minutes, add 0.3ml bromoacetyl bromide dropwise, and add NaHCO dropwise at the same time 3 solution (5%) until the system is completely clear. After reacting for 2 hours, the water phase was separated, and the pH of the water phase was adjusted to 1.0-1.5 with 6 mol / l hydrochloric acid, and a large amount of precipitation was p...
Embodiment 2
[0059] Preparation of intermediate 7-bromoacetamido-3-chloro-3-cephem-4-carboxylic acid
[0060] First add 2.34g of 7-amino-3-chloro-3-cephem-4-carboxylic acid to 30mlH 2 O, then add 30ml CH 2 Cl 2 . Stir in an ice-water bath, and when the temperature drops to 0-5°C, slowly add 1.15ml of tetramethylguanidine dropwise, and the 7-amino-3-chloro-3-cephem-4-carboxylic acid in the system is completely dissolved. Then add bromoacetyl bromide dropwise in batches, first add 0.8ml bromoacetyl bromide dropwise, stir rapidly, raise the temperature to 25-30°C, and at the same time add triethylamine dropwise until the system is completely clear; after 20 minutes, add 0.3ml bromoacetyl bromide dropwise Bromine, while adding triethylamine dropwise until the system is completely clear. After reacting for 2 hours, the water phase was separated, and the pH of the water phase was adjusted to 1.0-1.5 with 6 mol / l hydrochloric acid, and a large amount of precipitation was precipitated. After ...
Embodiment 3
[0065] Preparation of intermediate 7-bromoacetamido-3-chloro-3-cephem-4-carboxylic acid
[0066] First add 2.34g of 7-amino-3-chloro-3-cephem-4-carboxylic acid to 30mlH 2 O, then add 30ml acetone. Stir in an ice-water bath, and when the temperature drops to 0-5°C, add 0.75ml of ammonia water (25%), and the 7-amino-3-chloro-3-cephem-4-carboxylic acid in the system is completely dissolved. Then add bromoacetyl bromide dropwise in batches, first add 0.8ml bromoacetyl bromide dropwise, stir rapidly, raise the temperature to 25-30°C, and at the same time add diethylamine dropwise until the system is completely clear; after 20 minutes, add 0.3ml bromoacetyl bromide dropwise bromine, while adding diethylamine dropwise until the system is completely clear. After reacting for 2 hours, the water phase was separated, and the pH of the water phase was adjusted to 1.0-1.5 with 6 mol / l hydrochloric acid, and a large amount of precipitation was precipitated. After growing crystals in an i...
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