Preparation method of intermediate of olprinone hydrochloride
A technology for oprenone and intermediates, which is applied in the field of preparation of key intermediates of the cardiotonic drug oprenone hydrochloride, can solve problems such as no relevant literature reports, and achieve stable and reproducible processes, high product purity, The effect of easy industrialization
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example 1
[0017] Example 1: Add 1140 grams of bromoacetaldehyde diethyl acetal and 5 liters of n-butanol to a 10-liter reactor equipped with a reflux device, 200 ml of concentrated hydrochloric acid, stir and raise the temperature, control the temperature at 60-80°C for 2 hours, and slowly add 500 gram of 2-amino-5-bromo-pyridine, react at a temperature of 80°C for 20 hours, stop heating, spin off the solvent, cool naturally, and precipitate a large amount of light yellow solid; filter with suction, add saturated sodium bicarbonate solution to dissolve the filter cake; extract with chloroform, organic The phase was washed with saturated brine; the organic phase was dried with anhydrous magnesium sulfate and filtered; to obtain a light red oil, add 1L of petroleum ether and stir at room temperature to obtain a large amount of white solid; filter the solid with air at 50°C to obtain a white solid product 498g, yield 87.7%. m / e: 197.85, 1H-NMR (300 M Hz, CDCl3) δ (ppm): 7.19 (1H, dd, J=2, ...
example 2
[0018] Example 2: Add 1140 grams of bromoacetaldehyde diethyl acetal and 5 liters of n-butanol to a 10-liter reactor equipped with a reflux device, 200 ml of concentrated hydrochloric acid, stir and raise the temperature, control the temperature at 60-80°C for 2 hours, and slowly add 500 gram of 2-amino-5-bromo-pyridine, reacted at 60°C for 24 hours, stopped heating, spun off the solvent, cooled naturally, and precipitated a large amount of light yellow solid; suction filtered, and the filter cake was dissolved by adding saturated sodium bicarbonate solution; extracted with chloroform, organic The phase was washed with saturated brine; the organic phase was dried with anhydrous magnesium sulfate and filtered; to obtain a light red oil, add 1L of petroleum ether and stir at room temperature to obtain a large amount of white solid; filter the solid with air at 50°C to obtain a white solid product 463g, yield 81.5%.
example 3
[0019] Example 3: Add 1140 grams of bromoacetaldehyde diethyl acetal and 5 liters of n-butanol to a 10-liter reactor equipped with a reflux device, 200 ml of concentrated hydrochloric acid, stir and raise the temperature, control the temperature at 60-80°C for 2 hours, and slowly add 500 gram of 2-amino-5-bromo-pyridine, reacted at 100°C for 72 hours, stopped heating, removed the solvent, cooled naturally, and precipitated a large amount of brown-yellow solid; suction filtered, and the filter cake was dissolved by adding saturated sodium bicarbonate solution; extracted with chloroform, organic The phase was washed with saturated brine; the organic phase was dried with anhydrous magnesium sulfate and filtered; to obtain a light red oil, add 1L of petroleum ether and stir at room temperature to obtain a large amount of white solid; filter the solid with air at 50°C to obtain a white solid product 396g, yield 69.7%.
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