Preparation technology avoiding reduction of tetracycline hydrochloride technical original drug property
A technology of tetracycline hydrochloride and preparation process, applied in the field of medicine, can solve the problems such as the reduction of the efficacy of the original tetracycline hydrochloride, and achieve the effects of avoiding the reduction of the efficacy of the original tetracycline hydrochloride and the performance damage.
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Embodiment 1
[0023] Such as figure 1 Shown, avoid reducing the preparation technology of the original drug property of tetracycline hydrochloride, comprise the following steps:
[0024] 1) Preparation of tetracycline hydrochloride: Mix tetracycline hydrochloride urea double salt with organic alcohol mixed solvent at a ratio of 1g: 6mL, stir continuously at 10°C for 10 minutes, add hydrochloric acid, and filter after continuous stirring; transfer the obtained filtrate into a crystallizer After heating up, add seed crystals when the system temperature reaches 30°C, continue to heat up to 45°C, and incubate at a constant temperature for 30 minutes; then lower the temperature of the suspension to 10°C at a cooling rate of 5°C / min; filter the obtained crystal slurry, wash with a solvent, Obtain tetracycline hydrochloride crystal product; The mol ratio of effective HCl in described tetracycline hydrochloride urea double salt and hydrochloric acid is 1:1; Described organic solvent mixed agent is ...
Embodiment 2
[0028] Such as figure 1 Shown, avoid reducing the preparation technology of the original drug property of tetracycline hydrochloride, comprise the following steps:
[0029] 1) Preparation of tetracycline hydrochloride: Mix tetracycline hydrochloride urea double salt with organic alcohol mixed solvent in a ratio of 1g: 8mL, stir continuously at 15°C for 10min, add hydrochloric acid, and filter after continuous stirring; transfer the obtained filtrate into a crystallizer After the temperature rises, when the system temperature reaches 35°C, add seed crystals, continue to heat up to 50°C, and incubate at a constant temperature for 30 minutes; then lower the temperature of the suspension to 15°C at a rate of 8°C / min; filter the obtained crystal slurry, and wash with a solvent. Obtain tetracycline hydrochloride crystal product; The mol ratio of effective HCl in described tetracycline hydrochloride urea double salt and hydrochloric acid is 1:2; Described organic solvent mixture is t...
Embodiment 3
[0033] Such as figure 1 Shown, avoid reducing the preparation technology of the original drug property of tetracycline hydrochloride, comprise the following steps:
[0034]1) Preparation of tetracycline hydrochloride: Mix tetracycline hydrochloride urea double salt with organic alcohol mixed solvent in a ratio of 1g: 10mL, stir continuously at 18°C for 10min, add hydrochloric acid, and filter after continuous stirring; transfer the obtained filtrate into a crystallizer After heating up, add seed crystals when the system temperature reaches 35°C, continue to heat up to 48°C, and incubate at a constant temperature for 30 minutes; then lower the temperature of the suspension to 18°C at a cooling rate of 6°C / min; filter the obtained crystal slurry, wash with a solvent, Obtain tetracycline hydrochloride crystal product; The mol ratio of effective HCl in described tetracycline hydrochloride urea double salt and hydrochloric acid is 1:2; Described organic solvent mixture is the m...
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