Medetomidine industrial splitting method
A technology of medetomidine and imidazole, which is applied in the field of industrial separation of medetomidine, can solve the problem of low resolution yield and achieve the effect of simple industrial operation and high efficiency
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Embodiment 1
[0027] Example 1: Preparation of (S)-medetomidine L-(-)camphorsulfonate
[0028] Add 400g (2.0mol) of medetomidine, 10L of absolute ethanol, 233g (1.0mol) of L-(-)camphorsulfonic acid into a 20L reactor, stir and heat up, dissolve and reflux at 75±5°C for 20min, and the temperature will drop naturally Crystallize at 5±2°C for 18h. Suction filtration, 300% absolute ethanol slurry washing, filter drying, the filter cake was dried under vacuum at 50°C for 5h to obtain 415g of white solid (S)-medetomidine L-(-)camphorsulfonate, yield 46%, optical purity 99.6%.
Embodiment 2
[0029] Example 2: Preparation of (S)-medetomidine L-(-)camphorsulfonate
[0030] Add 400g (2.0mol) of medetomidine, 12L of absolute ethanol, and 345g (1.5mol) of L-(-) camphorsulfonic acid into a 20L reactor, stir and heat up, dissolve and reflux at 75±5°C for 20min, and the temperature will drop naturally Crystallize at 5±2°C for 18h. Suction filtration, 350% ethanol slurry washing, filter drying, filter cake 50 ℃ vacuum drying for 5h to obtain white solid (S)-medetomidine L-(-)camphorsulfonate 419g, yield 46.7%, optical purity 99.8%.
Embodiment 3
[0031] Example 3: The preparation of dexmedetomidine hydrochloride
[0032] Put 3500ml of dichloromethane, 2000ml of water, and 200g of the compound of Example 1 into a 10L reaction bottle, stir and dissolve, adjust the pH value to 9±1 with concentrated ammonia water, let it stand and separate after the pH value is stable, wash the organic phase with 700ml×2 water, Stir with anhydrous sodium sulfate until clear, dry for 3 hours, filter with suction, rinse the filter cake with 500ml of dichloromethane, combine the mother liquors, and evaporate to dryness under reduced pressure at 40±5°C to obtain a white solid. The obtained white solid was dissolved in 1500ml of dichloromethane, 87ml of 10N ethanol hydrochloric acid solution was added dropwise, stirred for 20min, and then 6000ml of anhydrous ether was quickly dropped into, stirred and crystallized for 5h. Suction filtration, wash the filter cake with anhydrous diethyl ether slurry, and dry the filter cake at 60°C for 6 hours ...
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