A kind of preparation method of cefozopram hydrochloride
A technology for cefazolam hydrochloride and cefazolam, which is applied in the field of preparation of cefazolam hydrochloride and can solve the problems of high solvent residue and moisture content
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Embodiment 1
[0033]Embodiment 1: the preparation of cefozopran hydrochloride
[0034] Method 1: Preparation of Cefozopran Hydrochloride by Ordinary Conventional Methods
[0035] Add 40 g of the intermediate cefozopran into a 250 ml reaction flask, add 70 ml of acetone, 40 ml of water and 30 ml of 12N HCl under stirring at 30°C, stir and dissolve for 4 hours, decolorize with activated carbon. The filtrate was transferred to a 1L reaction flask, 200ml of acetone was added, stirred for 4h, then 500ml of acetone was added dropwise, and the crystal was grown for 2h. Suction filtration, the filter cake was washed with acetone, and vacuum-dried at 45°C to obtain 31.1 g of the product with a yield of 72.4%, a purity of 99.6% by HPLC, acetone solvent residue of 4.5%, and a moisture content of 4.2%.
[0036] Method two: Utilize the technical scheme of the present invention to prepare Cefozopran Hydrochloride:
[0037] (1) Add 40 g of the intermediate cefozopran into a 250 ml reaction flask, add 70...
Embodiment 2
[0043] Embodiment 2: the preparation of cefozopran hydrochloride
[0044] Method 1: Preparation method of common cefozopran hydrochloride:
[0045] Add 40 g of cefozopran into a 250 ml reaction bottle, add 70 ml of acetone, 40 ml of water and 30 ml of 12N HCl under stirring at 32°C, stir to dissolve, and decolorize the activated carbon. The filtrate was transferred to a 1L reaction flask, 200ml of acetone was added, stirred for 2h, then 500ml of acetone was added dropwise, and the crystal was grown for 2h. After suction filtration, the filter cake was washed with acetone and dried in vacuo at 45°C to obtain 30.8 g of acetone solvate with a yield of 72.0%, a purity of 99.5% by HPLC, acetone solvent residue of 4.3%, and a water content of 4.3%.
[0046] Method two: Utilize the technical scheme of the present invention to prepare Cefozopran Hydrochloride:
[0047] (1) Add 40 g of cefozopran into a 250 ml reaction bottle, and add 40 ml of acetone, 30 ml of ethanol, 40 ml of wate...
Embodiment 3
[0052] Embodiment 3: the preparation of cefozopran hydrochloride
[0053] Method 1: Preparation method of common cefozopran hydrochloride:
[0054] Add 40 g of cefozopran into a 250 ml reaction bottle, add 70 ml of acetone, 40 ml of water and 30 ml of 12N HCl under stirring at 35°C, stir to dissolve, and decolorize the activated carbon. The filtrate was transferred to a 1L reaction flask, 200ml of acetone was added, stirred for 2h, then 500ml of acetone was added dropwise, and the crystal was grown for 2h. After suction filtration, the filter cake was washed with acetone and dried in vacuo at 45°C to obtain 31.0 g of acetone solvate with a yield of 72.4%, a purity of 99.3% by HPLC, acetone solvent residue of 4.5%, and a water content of 4.3%.
[0055] Method two: Utilize the technical scheme of the present invention to prepare Cefozopran Hydrochloride:
[0056] (1) Add 40 g of cefozopran into a 250 ml reaction flask, and add 50 ml of acetone, 20 ml of methanol, 40 ml of wate...
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