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Synthetic method of isoproterenol drug intermediate 2,4-dyhydroxy-alpha-chloroacetophenone
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A technology of isoproterenol and chloroacetophenone, applied in the field of isoproterenol pharmaceutical intermediate 2, can solve problems such as low selectivity, improve reaction yield, reduce intermediate links, reduce reaction temperature and reaction effect of time
Inactive Publication Date: 2017-02-22
XIAMEN AN PU DUN INFORMATION TECH CO LTD
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Mainly stimulates β receptors, has low selectivity for β1 and β2 receptors, and has little effect on α receptors
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example 1
[0011] Add 0.13mol of resorcinol (2), 15ml of chloroacetamide (3), and 80ml of nitromethane into the reaction vessel, lower the temperature of the solution to 3°C, control the stirring speed at 120rpm, add 0.021mol of cuprous chloride, and add mass The fraction is 30% oxalic acid solution 300ml, let stand for 36h, the solution is layered, the nitromethane layer is poured out, the mass fraction is 70% ethyl acetate, wash 3 times, add 600ml mass fraction is 10% potassiumchloride solution, reflux reaction 3h, standing still for 30h, the solid precipitated, suction filtered, the solid was washed successively with sodiumbromide solution, the mass fraction was 70% chlorobenzene, and recrystallized in 95% toluene to obtain yellow needle-like crystal 2,4- Dihydroxy-α-chloroacetophenone 12.64g, yield 52%.
example 2
[0013] Add 0.13mol of resorcinol (2), 16ml of chloroacetamide (3), and 80ml of nitromethane into the reaction vessel, lower the temperature of the solution to 4°C, control the stirring speed at 130rpm, add 0.022mol of cuprous chloride, add mass The fraction is 33% oxalic acid solution 300ml, let stand for 36h, the solution is layered, pour off the nitromethane layer, wash with 72% ethyl acetate for 4 times, add 600ml mass fraction of 12% potassium chloride solution, reflux reaction 3h, standing still for 33h, the solid precipitated, suction filtered, the solid was washed successively with potassium sulfate solution, the mass fraction was 72% chlorobenzene, and recrystallized in 96% toluene to obtain yellow needle-like crystals of 2,4-di Hydroxy-α-chloroacetophenone 13.86g, yield 57%.
example 3
[0015] Add 0.13mol of resorcinol (2), 17ml of chloroacetamide (3), and 80ml of nitromethane into the reaction vessel, lower the temperature of the solution to 5°C, control the stirring speed at 150rpm, add 0.023mol of cuprous chloride, add mass The fraction is 35% oxalic acid solution 300ml, let stand for 36h, the solution is layered, the nitromethane layer is poured out, the mass fraction is 75% ethyl acetate, wash 5 times, add 600ml mass fraction is 15% potassium chloride solution, reflux reaction 4h, standing still for 35h, the solid precipitated, suction filtered, the solid was washed successively with sodiumbromide solution, the mass fraction was 75% chlorobenzene, and recrystallized in 98% toluene to obtain yellow needle-like crystal 2,4- Dihydroxy-α-chloroacetophenone 15.07g, yield 62%.
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Abstract
The invention relates to a synthetic method of isoproterenol drug intermediate 2,4-dyhydroxy-alpha-chloroacetophenone. The synthetic method includes the following steps that 0.13 mol of resorcinol, 15-17 ml of chloroacetamide and 80 ml of nitromethane are added into a reaction container, the solution temperature is reduced to 3-5 DEG C, the stirring speed is controlled to be 120-150 rpm, 0.021-0.023 mol of cuprous chloride and 300 ml of oxalic acid solution are added, the solution is layered after carrying out standing still for 36 h, the nitromethane layer is poured out, ethyl acetate is used for washing for 3-5 times, 600 ml of potassiumchloride solution is added, reflux reaction is carried out for 3-4 h, solid is separated after carrying out standing still for 30-35 h, suction filtration is carried out, and the solid is sequentially washed with salt solution and chlorobenzene and recrystallized in methylbenzene to obtain yellow needle-like crystal 2,4-dyhydroxy-alpha-chloroacetophenone; the mass fraction of the oxalic acid solution, the mass fraction of ethyl acetate and the mass fraction of potassiumchloride solution are 30-35%, 70-75% and 10-15% respectively.
Description
technical field [0001] The invention relates to a method for synthesizing isoproterenol drug intermediate 2,4-dihydroxy-alpha-chloroacetophenone. Background technique [0002] Isoproterenol is mainly used to treat bronchial asthma, and is suitable for controlling acute attacks of asthma. It is often administered by aerosolinhalation, and its effect is fast and strong, but the duration is short. Cardiac arrest, used to treat cardiac arrest caused by various reasons such as drowning, electric shock, surgical accident and drug poisoning. When necessary, it can be combined with epinephrine and norepinephrine. Atrioventricular block. Anti-shock, can be used for cardiogenic shock and septic shock. For those with high central venous pressure and low cardiac output, this product should be used on the basis of replenishing blood volume. It mainly stimulates β receptors, has low selectivity for β1 and β2 receptors, and has almost no effect on α receptors. Bronchodilator: acts on...
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