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Organic synthesis intermediate acetone oxime synthesis method

A technology of organic synthesis and synthesis method, applied in the direction of organic chemistry, oxime preparation, etc., can solve the problems of complex process and low final yield, and achieve the effect of reducing intermediate links, shortening reaction time, and improving reaction yield

Inactive Publication Date: 2018-06-26
CHENGDU KA DI FU TECH
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Problems solved by technology

[0002] Acetone oxime is mainly used as an intermediate in organic synthesis, and can also be used in the identification process of metal ions such as nickel and cobalt. Its aqueous solution is neutral and can discolor potassium permanganate at room temperature. It is mainly used for chemical removal of feed water in industrial boilers. Oxygen agent, compared with traditional boiler chemical oxygen scavenger, has the characteristics of less dosage, high oxygen scavenging efficiency, non-toxic, and non-polluting environment. It is the best drug for shutdown protection and passivation treatment of critical boilers. However, Most of the existing synthetic methods adopt sodium hydroxide as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which will further improve the quality and yield of the product, reduce the By-product content is economically important

Method used

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  • Organic synthesis intermediate acetone oxime synthesis method

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Effect test

example 1

[0011] Dissolve 0.5 mol of hydroxylamine phosphate in 20 L of potassium chloride solution with a mass fraction of 15%, slowly add 0.6 mol of acetone solution with a mass fraction of 30%, control the solution temperature at 35°C, let it stand for 90 minutes after adding, and lower the solution temperature to 31 ℃, add 0.9mol mass fraction of 20% potassium bicarbonate solution to adjust the pH of the solution to 8.5, control the solution temperature to 41 °C, separate the layers after cooling, separate the oil layer, and distill under reduced pressure at 50kPa to collect the fraction at 90 °C, the mass fraction Wash with 70% cyclohexane solution, wash with 90% isopropanol solution by mass fraction, dehydrate with anhydrous potassium carbonate dehydrating agent, cool and crystallize to obtain 33.215 g of finished acetone oxime with a yield of 91%.

example 2

[0013] Dissolve 0.5 mol of hydroxylamine phosphate in 20 L of potassium chloride solution with a mass fraction of 17%, slowly add 0.7 mol of acetone solution with a mass fraction of 32%, control the solution temperature at 37°C, let it stand for 100 minutes after adding, and lower the solution temperature to 32 ℃, add 0.9mol mass fraction of 22% potassium bicarbonate solution to adjust the pH value of the solution to 8.7, control the solution temperature to 43 ℃, separate the layers after cooling, separate the oil layer, distill under reduced pressure at 53kPa, collect the fraction at 93 ℃, the mass fraction Wash with 72% cyclohexane solution, wash with 93% isopropanol solution by mass fraction, dehydrate with anhydrous calcium sulfate dehydrating agent, cool and crystallize to obtain 33.945 g of finished acetone oxime with a yield of 93%.

example 3

[0015] Dissolve 0.5 mol of hydroxylamine phosphate in 20 L of potassium chloride solution with a mass fraction of 20%, slowly add 0.8 mol of acetone solution with a mass fraction of 35%, control the solution temperature at 39°C, let it stand for 110min after adding, and lower the solution temperature to 34 ℃, adding 0.9 mol mass fraction of 25% potassium bicarbonate solution to adjust the pH value of the solution to 9, controlling the solution temperature to 45 ℃, stratifying after cooling, separating the oil layer, distilling under reduced pressure at 55kPa, collecting the fraction at 95 ℃, mass fraction Wash with 75% cyclohexane solution, wash with 96% isopropanol solution by mass fraction, dehydrate with anhydrous potassium carbonate dehydrating agent, cool and crystallize to obtain 35.04 g of finished acetone oxime with a yield of 96%.

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Abstract

The invention relates to an organic synthesis intermediate acetone oxime synthesis method, which mainly comprises: dissolving 0.5 mol hydroxylamine phosphate in 20 L of a potassium chloride solution,slowly adding 0.6-0.8 mol of an acetone solution, controlling the solution temperature at 35-39 DEG C, standing for 90-110 min after the adding, reducing the solution temperature to 31-34 DEG C, adding 0.9 mol of a potassium bicarbonate solution, adjusting the pH value of the solution to 8.5-9, controlling the solution temperature at 41-45 DEG C, layering after cooling, extracting the obtained oillayer, carrying out pressure reducing distillation, collecting the distillate at a temperature of 90-95 DEG C, washing with a cyclohexane solution, washing with an isopropanol solution, dehydrating with a dehydrating agent, and carrying out cooling crystallization to obtain the finished product acetone oxime.

Description

technical field [0001] The invention relates to a method for synthesizing an organic synthesis intermediate acetone oxime. Background technique [0002] Acetone oxime is mainly used as an intermediate in organic synthesis, and can also be used in the identification process of metal ions such as nickel and cobalt. Its aqueous solution is neutral and can discolor potassium permanganate at room temperature. It is mainly used for chemical removal of feed water in industrial boilers. Oxygen agent, compared with traditional boiler chemical oxygen scavenger, has the characteristics of less dosage, high oxygen scavenging efficiency, non-toxic, and non-polluting environment. It is the best drug for shutdown protection and passivation treatment of critical boilers. However, Most of the existing synthetic methods adopt sodium hydroxide as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, wh...

Claims

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Application Information

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IPC IPC(8): C07C251/38C07C249/08
CPCC07C249/08C07C251/38
Inventor 廖如佴
Owner CHENGDU KA DI FU TECH
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