* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With hydrogenchloride In methanol at 0 - 5℃; for 1 h;
Moxifloxacin base 50.0 g was stirred in 200.0 ml methanol for 10-15 minutes at 25-3-0C. The pH was adjusted to 1.0 -2.0 using methanolic hydrochloric acid. The reaction mass was chilled to 0-50C and maintained for 1 hour. The solids were filtered and dried under vacuum at 85-900C to yield 52.5 g (105percent) of moxifloxacin hydrochloride; 70.0 g of moxifloxacin base was stirred with 350.0 ml of methanol at 25- 30°. The pH was adjusted to 1.0 - 2.0 using methanolic hydrochloric acid and contents were chilled to 0-5°C and stirred for 1 hour at the same temperature. The solid was filtered and dried under vacuum at 85-9O°C to yield 78.Og (77percent) of moxifloxacin hydrochloride
54.84%
With hydrogenchloride; edetate disodium In methanol; water at 0 - 38℃; for 2 h;
The compound obtained from the example 6(85g) was taken in methanol (250 ml) and purified water (150 ml) followed by the addition of hydrochloric acid (17.14 g) and EDTA disodium salt (57 mg) the contents was heated to 35-38°C and maintained for 1 hour ,cooled to 0-5°C for 1 hour. The product was filtered washed with methanol treated with activated carbon (5.0 g) to get the desired product. Dry wt: 53.0g, Yield: 54.84percent
44.3 g
With hydrogenchloride In ethanol; water at 20 - 60℃; for 6 h;
68.2 g of purified Moxifloxacin Tosylate of example 2 (1.0 mol. Equiv.) (HPLC purity equivalent to 99.30percent and impurity of formula (VII) equivalent to 0.27percent), 409.2 mL of saturated NaHCO3 solution, 136.4 mL of purified water, 409.2 mL of dichloromethane and 68.2 mL of isopropanol were introduced into a 4-neck flask provided with a mechanical stirrer, thermometer, cooler and thermostat. Heating is carried out at 30-35°C and stirring is carried out for one hour up to complete dissolution. Then the phases are separated and the aqueous phase is extracted using 136.4 mL of Dichloromethane. The organic phases are collected and dried. The obtained solid is recovered with 954.8 mL of Ethanol and 136.4 mL of purified water. Heating is carried out at reflux up to complete dissolution, then it is brought to 60°C and a solution of 12.3 mL of concentrated hydrochloric acid (32percent) (1.05 mol. equiv.) and 136.4 mL of Ethanol is dripped in 2 hours. It is brought to r.t in 4 hours, it is left at room temperature for at least 4 hours, then it is cooled at 0°C and it is left at 0°C for another 4 hours. The obtained crystal is filtered washing it with 68.2 mL of Ethanol. The obtained salt is dried at 50°C under vacuum for 24 hours. 44.3 g of Moxifloxacin hydrochloride with a molar yield equivalent to 85.1percent with HPLC purity equivalent to 99.79percent and a formula (VII) impurity content equivalent to 0.08percent are obtained. The obtained product does not contain, even at ppm level, any ester of the sulfonic acids as an impurity, which is an essential aspect it being widely known that such impurities are genotoxic.#10;
44.3 g
With hydrogenchloride In ethanol; water at 20 - 60℃; for 10 h;
68.2 g of purified moxifloxacin tosylate of example 2 (1.0 mol. Equiv.) (HPLC purity equivalent to 99.30percent and impurity of formula (VII) equivalent to 0.27percent), 409.2 mL of saturated NaHCO3 solution, 136.4 mL of purified water, 409.2 mL of dichloromethane and 68.2 mL of isopropanol were introduced into a 4-neck flask provided with a mechanical stirrer, thermometer, cooler and thermostat. Heating was carried out at 30-35°C and stirring was carried out for one hour up to complete dissolution. Then the phases were separated and the aqueous phase was extracted using 136.4 mL of Dichloromethane. The organic phases were collected and dried. The obtained solid was recovered with 954.8 mL of Ethanol and 136.4 mL of purified water. Heating was carried out at reflux up to complete dissolution, then it was brought to 60°C and a solution of 12.3 mL of concentrated hydrochloric acid (32percent) (1.05 mol. equiv.) and 136.4 mL of Ethanol was dripped in 2 hours. It was brought to r.t in 4 hours, it was left at room temperature for at least 4 hours, then it was cooled at 0°C and it was left at 0°C for another 4 hours. The obtained crystal was filtered washing it with 68.2 mL of Ethanol. The obtained salt was dried at 50° C. under vacuum for 24 hours. 44.3 g of moxifloxacin hydrochloride with a molar yield equivalent to 85.1percent with HPLC purity equivalent to 99.79percent and a formula (VII) impurity content equivalent to 0.08percent was obtained. The obtained product does not contain, even at ppm level, any ester of sulfonic acids as an impurity. This is important because it is well-known that such impurities are genotoxic.
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