Method for preparing high-purity 5-oxy(p-nitrobenzoyl)-nemadectin
A technology for nitrobenzoyl and nitrobenzoyl chloride is applied in the field of pharmaceutical chemical synthesis, and can solve the problems of high cost, many separation and purification steps, large solvent consumption and the like, and achieves low cost, improved purity and short production cycle. Effect
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Embodiment 1
[0025] Put crude 5-oxo(p-nitrobenzoyl)-nimoctine (20 g, purity 88.7%) and 20 mL of methanol into a 250 mL round bottom flask, raise the temperature to 60°C, and stir until it dissolves. 120 mL of deionized water was added dropwise, and then the temperature was lowered by a program of 6 °C per hour, and the temperature was lowered to 15 °C, filtered, and the filter cake was rinsed with 15 °C deionized water. The filter cake was vacuum-dried at 80°C for 20 h to obtain 15 g of high-purity 5-oxo(p-nitrobenzoyl)-nimoctine with a purity of 94.5%.
Embodiment 2
[0027] Put crude 5-oxo(p-nitrobenzoyl)-nimoctine (20 g, purity 88.7%) and 20 mL of n-propanol into a 250 mL round bottom flask, heat up to 80°C, and stir until dissolved. 100 mL of deionized water was added dropwise, and then the temperature was lowered by program, 4 °C per hour, and the temperature was lowered to 10 °C, filtered, and the filter cake was rinsed with 10 °C deionized water. The filter cake was vacuum-dried at 80°C for 20 h to obtain 14.4 g of high-purity 5-oxo(p-nitrobenzoyl)-nimoctine with a purity of 95.4%.
Embodiment 3
[0029] Put crude 5-oxo(p-nitrobenzoyl)-nimoctine (20g, purity 88.7%) and 14mL isopropanol into a 250 mL round bottom flask, heat up to 80°C, and stir until dissolved. 140 mL of deionized water was added dropwise, and then the temperature was lowered by 6 °C per hour, and the temperature was lowered to 10 °C, filtered, and the filter cake was rinsed with 10 °C deionized water. The filter cake was vacuum-dried at 80°C for 20 hours to obtain 16.7 g of high-purity 5-oxo(p-nitrobenzoyl)-nimoctine with a purity of 92.6%.
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