Deuterated alprazolam and preparation method thereof
A technology of deuterated alprazolam and alprazolam, which is applied in the field of deuterated alprazolam standard products and its preparation, can solve the problems of restricting wide use and high price, and achieve convenient operation, low cost and easy preparation The effect of the short method
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Embodiment 1
[0025] In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with magnetic force, then add 154mg, 0.5mmol non-deuterated alprazolam into the three-necked flask, and then add 10mL N, N-dimethylformamide , stirred at room temperature for 30 minutes to fully dissolve it, then added 138 mg of powdered potassium carbonate and 1 milliliter of deuterated chloroform in the three-necked flask, and replaced the three-necked flask with nitrogen three times at this time to remove air and moisture in the three-necked flask, and then placed the three-necked flask In an oil bath, raise the temperature to 120 degrees Celsius, stir and react for 2 hours, turn off the oil bath, place the reaction flask at room temperature to cool, and after cooling to room temperature, add 20 ml of water to the three-necked flask. At this time, the mixed liquid in the three-necked flask Transfer to a 100mL separatory funnel, and add 20mL of ethyl acetate to the separatory funnel. After ...
Embodiment 2
[0030] Embodiment 2 (comparative example)
[0031]In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with magnetic force, then add non-deuterated alprazolam (154mg, 0.5mmol) into the three-necked flask, and then add 10mL N, N-dimethyl Dimethyl formamide, stirred at room temperature for 30 minutes to make it fully dissolved, then added 138 mg of powdered potassium carbonate and 1 milliliter of deuterated chloroform in the three-necked flask, and now the three-necked flask was replaced with nitrogen three times to remove air and moisture in the three-necked flask, and then After the three-necked flask was stirred at room temperature for 24 hours, 20 ml of water was added to the three-necked flask. At this time, the mixed solution in the three-necked flask was transferred to a 100 mL separating funnel, and 20 mL of ethyl acetate was added to the separating funnel, and the mixture was shaken fully. After uniformity, let stand to separate the layers, se...
Embodiment 3
[0033] In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with magnetic force, then add non-deuterated alprazolam (154mg, 0.5mmol) into the three-necked flask, and then add 10mL N, N-dimethyl Dimethyl formamide, stirred at room temperature for 30 minutes to make it fully dissolved, then added 138 mg of powdered potassium carbonate and 0.5 milliliters of deuterated chloroform in the three-necked flask, and now the three-necked flask was replaced with nitrogen three times to remove air and moisture in the three-necked flask, and then The three-necked flask was placed in an oil bath, heated to 120 degrees Celsius, stirred and reacted for 6 hours, the oil bath was closed, and 20 milliliters of water was added to the three-necked flask. Add 20mL of ethyl acetate to the separatory funnel, shake it well, let stand to separate the layers, separate the ethyl acetate layer, continue to shake the water layer with 20mL of ethyl acetate to shake and extract, and...
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