Quinidine derivative and preparation method thereof
A technology of quinidine and derivatives, applied in the field of quinidine derivatives and its preparation
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Embodiment 1
[0018] Embodiment 1: The structural formula of the quinidine derivative is shown in formula I:
[0019] .
[0020] Above-mentioned derivative preparation method is as follows:
[0021] (1) Weigh 59 mg of sodium borohydride and place it in a 25 mL single-necked bottle, add 10 mL of anhydrous acetonitrile to it under nitrogen protection, cool in an ice bath for 5 minutes, and then add 195.4 mg of iodine. After the reaction solution turned from yellow to white, weigh 50 mg of quinidine and dissolve it in anhydrous acetonitrile, and slowly drop it into the reaction solution. After continuing to stir under the ice bath for 3 hours (after TLC monitored the reaction of quinidine), sodium hydroxide solution (2.3 mmol, 1 mol / L) was slowly added dropwise to the reaction solution, and the solution turned yellow, accompanied by a large amount of The gas is released, that is, hydrogen peroxide solution (3.08 mmol, mass percentage concentration is 35%) is added to the reaction liquid; t...
Embodiment 2
[0026] Embodiment 2: The structural formula of the quinidine derivative is shown in formula I:
[0027] .
[0028] The preparation method of quinidine derivative I is as follows:
[0029] (1) Weigh 50 mg of quinidine and dissolve it in 5 mL of anhydrous tetrahydrofuran, N 2 Cool to 0°C under protection, then add BH dropwise 3 THF (0.61 mmol, 1 mol / L) solution, continue stirring under ice bath for 4 hours (TLC monitors that the quinidine reaction is complete), slowly add sodium hydroxide solution (3.08 mmol, 1 mol / L) dropwise to the reaction solution L), the solution turned yellow, accompanied by a large amount of gas release, that is, hydrogen peroxide solution (3.85 mmol, 35% by mass percentage) was added to the reaction solution; the reaction system was slowly heated to 60 ° C for 1.5 hours, After the reaction solution was cooled to room temperature, it was extracted with chloroform, and the extract was washed with water and saturated brine successively, dried over anhy...
Embodiment 3
[0031] Embodiment 3: The structural formula of the quinidine derivative is shown in formula I:
[0032] .
[0033] The preparation method of quinidine derivative I is as follows:
[0034](1) Weigh 73.8 mg of sodium borohydride and place it in a 25 mL single-necked bottle, add 10 mL of anhydrous toluene to it under nitrogen protection, cool in an ice bath for 5 minutes, and then add 244.3 mg of iodine. After the reaction solution turns from yellow to white, weigh 50 mg of quinidine and dissolve it in anhydrous toluene, slowly drop it into the reaction solution, and continue to stir under ice bath for 3.5 hours (TLC monitors after the quinidine reaction is complete), Sodium hydroxide solution (2.85 mmol, 1 mol / L) was slowly added dropwise to the reaction solution, the solution turned yellow, accompanied by a large amount of gas evolution, that is, hydrogen peroxide solution (3.50 mmol, mass percent The concentration is 40%); the reaction system was slowly heated to 60°C for ...
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