Synthesis method of 9-demethyl-(+)-alpha-dihydrotetrabenazine
A technology of dihydrotetrabenazine and a synthetic method, which is applied in the direction of organic chemistry, can solve the problems of unfavorable large-scale industrial production, complex reaction operation, harsh reaction conditions, etc., and achieve short reaction time, simple reaction operation and low preparation cost. low effect
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Embodiment 1
[0043] The synthetic method of present embodiment 9-demethyl-(+)-α-dihydrotetrabenazine comprises the following steps:
[0044] Dissolve 1mmol of 9-benzyloxy-(+)-α-dihydrotetrabenazine in 5mL of methanol, add 2mmol of hydrobromic acid dropwise under stirring, and react at room temperature for 0.5h to obtain 9-desmethyl-(+ )-alpha-dihydrotetrabenazine crude product reaction solution;
[0045] It also includes the following steps of separation and purification treatment:
[0046](1) concentrating the reaction solution of the crude 9-desmethyl-(+)-α-dihydrotetrabenazine under reduced pressure to obtain a solid;
[0047] (2) Dissolving the solid in a mixed solvent of dichloromethane / ethyl acetate / methanol (volume ratio 1:1:0.05), standing still and crystallizing to obtain crystals;
[0048] (3) Dissolve the crystals in water, adjust the pH value to 7-9 with aqueous sodium hydroxide solution, extract with ether, and concentrate the organic phase under reduced pressure to obtain 9...
Embodiment 2
[0054] The synthetic method of present embodiment 9-demethyl-(+)-α-dihydrotetrabenazine comprises the following steps:
[0055] Dissolve 1mmol of 9-benzyloxy-(+)-α-dihydrotetrabenazine in 5mL of ethanol, add 5mmol of hydrobromic acid dropwise under stirring, and react for 1h at room temperature to obtain 9-desmethyl-(+) -The reaction liquid of α-dihydrotetrabenazine crude product;
[0056] It also includes the following steps of separation and purification treatment:
[0057] (1) concentrating the reaction solution of the crude 9-desmethyl-(+)-α-dihydrotetrabenazine under reduced pressure to obtain a solid;
[0058] (2) Dissolving the solid in a mixed solvent of dichloromethane / ethyl acetate / methanol (volume ratio 0.8:1.2:0.04), standing still and crystallizing to obtain crystals;
[0059] (3) Dissolve the crystals in water, adjust the pH value to 7-9 with potassium hydroxide aqueous solution, extract with ether, and concentrate the organic phase under reduced pressure to ob...
Embodiment 3
[0065] The synthetic method of present embodiment 9-demethyl-(+)-α-dihydrotetrabenazine comprises the following steps:
[0066] Dissolve 1mmol of 9-benzyloxy-(+)-α-dihydrotetrabenazine in 5mL of methanol, add 20mmol of hydrobromic acid dropwise under stirring, and react at room temperature for 1.5h to obtain 9-desmethyl-(+ )-alpha-dihydrotetrabenazine crude product reaction solution;
[0067] It also includes the following steps of separation and purification treatment:
[0068] (1) concentrating the reaction solution of the crude 9-desmethyl-(+)-α-dihydrotetrabenazine under reduced pressure to obtain a solid;
[0069] (2) Dissolving the solid in a mixed solvent of dichloromethane / ethyl acetate / methanol (volume ratio 1.2:0.8:0.06), standing still and crystallizing to obtain crystals;
[0070] (3) Dissolve the crystals in water, adjust the pH value to 7-9 with aqueous sodium carbonate solution, extract with ether, and concentrate the organic phase under reduced pressure to ob...
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