Preparation method of demebeverine hydrochloride
A technology of norephrine and hydrochloride, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxyl compounds, etc., and can solve the problems of safety and high price
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Embodiment 1
[0014] Add 5ml of methanol to a 50ml single-necked bottle, add 0.75g of sodium metal after cooling to 0°C, stir until dissolved to obtain sodium methoxide, slowly add 10ml of nitromethane dropwise at 0°C, after dropping, stir at 0°C for 15 minutes to form Light yellow negative ion suspension, then dissolve 1.0g, 8.2mmol of m-hydroxybenzaldehyde in 10ml of nitromethane, slowly drop into the negative ion suspension, slowly rise to room temperature, stir overnight, add saturated ammonium chloride solution to terminate the reaction , the reaction solution was extracted with ethyl acetate, the organic phases were combined, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated to obtain a light yellow oil, purified by column chromatography to obtain a light yellow solid intermediate 3-(1- Hydroxy-2-nitro)ethylphenol 1.104g, yield 73.6%, or 79.3% based on actual utilization of raw materials, and 72 mg of unreacted raw materials were recovered.
[0015] Add 20...
Embodiment 2
[0017] Add 10ml of nitromethane into a 50ml single-necked bottle, cool to 0°C, add 0.82g of solid potassium hydroxide 0.82g, 20.5mmol in batches, then add 2ml of anhydrous methanol, stir at 0°C for 60 minutes, and form a light yellow negative ion suspension solution, and then 1.0 g of m-hydroxybenzaldehyde, 8.2 mmol was dissolved in 10 ml of nitromethane, slowly added dropwise to the negative ion suspension, slowly raised to room temperature, stirred overnight, and saturated ammonium chloride solution was added to terminate the reaction, and ethyl acetate The reaction solution was extracted from the ester, the organic phases were combined, washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated to obtain a brownish yellow oil, which was purified by column chromatography to obtain a light yellow solid intermediate product 3-(1-hydroxyl-2- Nitro)ethylphenol 1.06g, 70.1%, or 76.7% based on the actual raw material yield, and 80 mg of unreacted raw materia...
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