A kind of preparation method of cefditoren pivoxil
A technology of cefditoren pivoxil and compounds, which is applied in the field of preparation of cephalosporins, can solve problems such as poor yield and strong corrosion of reagents, and achieve the effects of increased yield, high yield and simple process
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Embodiment 1
[0026] (6R,7R)-7-[(Z)-2-(2-aminothiazol-4-yl)-2-methoxyiminoacetamido]-3-[(Z)-2-(4-methyl Preparation of lithium-5-thiazolyl)vinyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate
[0027] Put 200g of 7-amino-3-[(Z)-2-(4-methyl-5-thiazolyl)vinyl]-3-cephem-4-carboxylic acid, 2-methoxyimino into the reaction flask - 240g of 2-(2-amino-4-thiazolyl)-(z)-benzothiazolyl thioacetate, 2000ml of dichloromethane, lower the temperature to 0°C, and add 120g of ethylamine dropwise. Add water, separate the layers, adjust the pH of the aqueous layer to 2.8 with dilute hydrochloric acid, and centrifuge until dry. The filter cake was completely dissolved with 5000ml of acetone, 130g of lithium tert-butoxide was added to react for 1 hour, filtered, and the product was dried to obtain 270g of the title compound with a yield of 80.0%.
Embodiment 2
[0029] Put 200g of 7-amino-3-[(Z)-2-(4-methyl-5-thiazolyl)vinyl]-3-cephem-4-carboxylic acid, 2-methoxyimino into the reaction flask - 240 g of 2-(2-amino-4-thiazolyl)-(z)-benzothiazolyl thioacetate, 2000 ml of dichloromethane, lower the temperature to 0°C, and add 145 g of triethylamine dropwise. Add water, separate the layers, adjust the pH of the aqueous layer to 2.8 with dilute hydrochloric acid, and centrifuge until dry. The filter cake was completely dissolved with 5000ml of acetone, 130g of lithium tert-butoxide was added to react for 1 hour, filtered, and the product was dried to obtain 276g of the title compound with a yield of 82.1%.
Embodiment 3
[0031] Put 200g of 7-amino-3-[(Z)-2-(4-methyl-5-thiazolyl)vinyl]-3-cephem-4-carboxylic acid, 2-methoxyimino into the reaction flask - 240 g of 2-(2-amino-4-thiazolyl)-(z)-benzothiazolyl thioacetate, 2000 ml of dichloromethane, lower the temperature to 0°C, and add 157 g of triethanolamine dropwise. Add water, separate the layers, adjust the pH of the aqueous layer to 2.8 with dilute hydrochloric acid, and centrifuge until dry. The filter cake was completely dissolved with 5000ml of acetone, 130g of lithium tert-butoxide was added to react for 1 hour, filtered, and the product was dried to obtain 254g of the title compound with a yield of 74.3%.
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