Deuterated triazolam and preparation method thereof
A technology of deuterated triazolam and triazole, applied in the field of deuterated triazolam standard product and preparation thereof, can solve the problems of limited use, high price, high cost and the like, and achieves convenient operation, low cost, preparation method short effect
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Embodiment 1
[0027]In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with a magnetic force, and then add 171 mg, 0.5 mmol of 8-chloro-6-(2-chlorophenyl)-1-methyl-4H to the three-necked flask -[1,2,4]triazolo[4,3-a][1,4]benzodiazepine, add 8mL dimethyl sulfoxide, stir at room temperature for 17 minutes to fully dissolve, then Add 326 mg of powdered cesium carbonate and 1 milliliter of deuterated chloroform in the three-necked flask. At this time, the three-necked flask is replaced with nitrogen three times to remove air and moisture in the three-necked flask. After this, the three-necked flask is placed in an oil bath, heated to 160 degrees Celsius, and stirred React for 1 hour, close the oil bath, place the reaction flask at room temperature to cool, add 20 ml of water to the three-necked flask after cooling to room temperature, and transfer the mixed solution in the three-necked flask to a 100mL separatory funnel, and pour it into the three-necked flask Add 2...
Embodiment 2
[0032] In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with a magnetic force, and then add 8-chloro-6-(2-chlorophenyl)-1-methyl-4H-[1 ,2,4]triazolo[4,3-a][1,4]benzodiazepine (171mg, 0.5mmol), add 8mL dimethyl sulfoxide, stir at room temperature for 17 minutes to fully Dissolve, then add powdered cesium carbonate 326mg and 1 milliliter of deuterated chloroform in the three-necked flask, now the three-necked flask is replaced three times with nitrogen, to remove air and moisture in the three-necked flask, after this the three-necked flask was stirred at room temperature for 24 hours, to Add 20 ml of water into the three-necked flask, at this time, transfer the mixed solution in the three-necked flask to a 100 mL separating funnel, and add 20 mL of n-butanol to the separating funnel. After the butanol layer, the water layer continued to be shaken and extracted with 20 mL of n-butanol, and the extraction was repeated 3 times. The n-butanol solutions...
Embodiment 3
[0034] In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with a magnetic force, and then add 8-chloro-6-(2-chlorophenyl)-1-methyl-4H-[1 ,2,4]triazolo[4,3-a][1,4]benzodiazepine (171mg, 0.5mmol), add 10mL dimethyl sulfoxide, stir at room temperature for 30 minutes to fully Dissolve, then add powdered cesium carbonate 326mg and 1 milliliter of deuterated chloroform in the three-necked flask, now the three-necked flask is replaced with nitrogen three times, to remove the air and moisture in the three-necked flask, after this the three-necked flask is placed in an oil bath, and the temperature is raised to 160 Celsius, stirred and reacted for 1 hour, closed the oil bath, and added 20 ml of water into 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 tert-butyl methyl ether was added to the separating funnel, fully After shaking and shaking, let stand to separat...
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