A kind of highly safe L-ornidazole injection and preparation method thereof
A technology for levornidazole and injection, which is applied in the directions of non-active ingredient medical preparations, active ingredients-containing medical preparations, pharmaceutical formulas, etc. Good performance and high purity
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Embodiment 1
[0052] In a 50L reaction kettle protected from light and under anaerobic conditions, add 20L ethyl acetate and 2kg of 2-methyl-5-nitroimidazole, cool down to -10°C, and slowly add boron trifluoride in ethyl acetate Ester solution (containing about 1.1kg of boron trifluoride) (control temperature not exceeding 15°C), after the dropwise addition, slowly add 2.2LS-(+)-epichlorohydrin (control temperature not exceeding 15°C), After dripping, react at 10°C for 5 hours, slowly add the reaction solution into 18kg of ice-water mixture, and stir the reaction for 5 hours at a temperature not exceeding 30°C, adjust the pH value to about 1.0 with concentrated hydrochloric acid, separate the organic layer, and use concentrated ammonia water for the water layer Adjust the pH to 7.0, stir and crystallize for 24 hours, filter, wash with water, and dry to obtain 3.21 kg of L-ornidazole.
[0053] Accurately weigh 83g of sodium chloride, 50g of L-ornidazole prepared by the above method, add 9000...
Embodiment 2
[0055] In a 50L reaction kettle protected from light and under anaerobic conditions, add 20L ethyl acetate and 2kg of 2-methyl-5-nitroimidazole, cool down to -10°C, and slowly add boron trifluoride in ethyl acetate Ester solution (containing about 1.1kg of boron trifluoride) (control temperature not exceeding 15°C), after the dropwise addition, slowly add 2.2LS-(+)-epichlorohydrin (control temperature not exceeding 15°C), After dripping, react at 10°C for 5 hours, slowly add the reaction solution into 18kg of ice-water mixture, and stir the reaction for 5 hours at a temperature not exceeding 30°C, adjust the pH value to about 1.0 with concentrated hydrochloric acid, separate the organic layer, and use concentrated ammonia water for the water layer Adjust the pH to 7.0, stir and crystallize for 24 hours, filter, wash with water, and dry to obtain 3.21 kg of L-ornidazole.
[0056] Accurately weigh 83g of sodium chloride, 50g of L-ornidazole prepared by the above method, and 0.05...
Embodiment 3
[0058] In a 50L reaction kettle protected from light and under anaerobic conditions, add 20L ethyl acetate and 2kg of 2-methyl-5-nitroimidazole, cool down to -10°C, and slowly add boron trifluoride in ethyl acetate Ester solution (containing about 1.1kg of boron trifluoride) (control temperature not exceeding 15°C), after the dropwise addition, slowly add 2.2LS-(+)-epichlorohydrin (control temperature not exceeding 15°C), After dripping, react at 10°C for 5 hours, slowly add the reaction solution into 18kg of ice-water mixture, and stir the reaction for 5 hours at a temperature not exceeding 30°C, adjust the pH value to about 1.0 with concentrated hydrochloric acid, separate the organic layer, and use concentrated ammonia water for the water layer Adjust the pH to 7.0, stir and crystallize for 24 hours, filter, wash with water, and dry to obtain 3.21 kg of L-ornidazole.
[0059] Under the conditions of 45 ℃, dark, and anaerobic protection, accurately weigh 83g of sodium chlori...
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