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Preparation method of acetaldoxime

A technology of acetaldehyde oxime and acetaldehyde, applied in the field of organic chemical synthesis, to achieve the effect of easy toxicity and safe use

Inactive Publication Date: 2019-03-01
江苏艾科维科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, acetaldehyde oxime is also an important organic synthesis reagent and analytical reagent. The acetaldehyde oxime used in organic synthesis must sometimes require anhydrous, but most of the acetaldehyde oxime provided in the domestic market is an aqueous solution with a content of about 40%, which cannot meet the needs. , providing a preparation of anhydrous acetaldoxime will have a good application prospect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of the acetaldehyde oxime of the present embodiment may further comprise the steps:

[0019] 1) Add hydroxylamine and distilled water to the four-necked flask equipped with electric stirring, dropping funnel, reflux condenser and thermometer to dissolve under stirring, then add acetaldehyde and catalyst acetic acid dropwise under ice-water bath cooling condition, add dropwise After completion, stir and react at 10° C. for 10 min to obtain an acetaldehyde oxime solution; the molar ratio of the hydroxylamine to distilled water is 1:1.05, and the mass ratio of the hydroxylamine to the distilled water is 1:1.1;

[0020] 2) Extract the acetaldehyde oxime solution in step 1) with 4 × 100ml dichloromethane, and after the extract is dried over anhydrous sodium sulfate, fractionate the dichloromethane at normal pressure, then distill under reduced pressure, and collect at a temperature of 76 ~ 78°C, pressure 2.0×10 4 The distillate at the time of Pa, obta...

Embodiment 2

[0023] The preparation method of the acetaldehyde oxime of the present embodiment may further comprise the steps:

[0024] 1) Add hydroxylamine and distilled water to the four-necked flask equipped with electric stirring, dropping funnel, reflux condenser and thermometer to dissolve under stirring, then add acetaldehyde and catalyst acetic acid dropwise under ice-water bath cooling condition, add dropwise After completion, stir and react at 8° C. for 20 minutes to obtain an acetaldehyde oxime solution; the molar ratio of the hydroxylamine to distilled water is 1:1.07, and the mass ratio of the hydroxylamine to the distilled water is 1:1.2;

[0025] 2) Extract the acetaldehyde oxime solution in step 1) with 4 × 100ml dichloromethane, and after the extract is dried over anhydrous sodium sulfate, fractionate the dichloromethane at normal pressure, then distill under reduced pressure, and collect at a temperature of 76 ~ 78°C, pressure 2.0×10 4 The distillate at the time of Pa, o...

Embodiment 3

[0028] The preparation method of the acetaldehyde oxime of the present embodiment may further comprise the steps:

[0029] 1) Add hydroxylamine and distilled water to the four-necked flask equipped with electric stirring, dropping funnel, reflux condenser and thermometer to dissolve under stirring, then add acetaldehyde and catalyst acetic acid dropwise under ice-water bath cooling condition, add dropwise After completion, stir and react at 9° C. for 30 min to obtain an acetaldehyde oxime solution; the molar ratio of the hydroxylamine to distilled water is 1:1.1, and the mass ratio of the hydroxylamine to the distilled water is 1:1.2;

[0030] 2) Extract the acetaldehyde oxime solution in step 1) with 4 × 100ml dichloromethane, and after the extract is dried over anhydrous sodium sulfate, fractionate the dichloromethane at normal pressure, then distill under reduced pressure, and collect at a temperature of 76 ~ 78°C, pressure 2.0×10 4 The distillate at the time of Pa, obtain...

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Abstract

The invention relates to the technical field of organic chemical synthesis, in particular to a preparation method of acetaldoxime. The preparation method of acetaldoxime includes the following steps of 1, stirring and dissolving hydroxylamine and distilled water, then adding acetaldehyde and catalytic acetic acid dropwise under an ice water bath condition, conducting stirring for a reaction at 0-10 DEG C for 10-30 minutes after the dropwise addition is completed, and then obtaining an acetaldoxime solution; 2, using dichloromethane for extracting the acetaldoxime solution in step 1, using anhydrous sodium sulfate for drying an extracted liquid, then conducting fractional distillation under normal pressure to obtain a solvent at first, conducting distillation under reduced pressure to collect fractions, and obtaining a colorless transparent liquid, namely acetaldoxime. The preparation method of acetaldoxime adopts acetic acid as a catalyst, hydroxylamine and acetaldehyde are adopted asraw materials to prepare the acetaldoxime solution, and then through extraction, drying, fractionation under normal pressure and distillation under reduced pressure, the colorless transparent liquid,namely acetaldoxime, is obtained. Obtained acetaldoxime is anhydrous, the purity is higher than or equal to 99%, and the yield is higher than or equal to 92%.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a preparation method of acetaldehyde oxime. Background technique [0002] Aldoxime is a reducing agent with low toxicity, a new type of oxygen scavenger with less pollution, low price and excellent oxygen scavenging effect. It is also an important organic synthesis and analysis reagent. In the 1990s, acetaldehyde oxime replaced the highly toxic hydrazine as a boiler water oxygen scavenger, and its oxygen scavenging effect was much higher than that of hydrazine, so it was widely used. Acetaldoxime is an important intermediate for the synthesis of pesticides methomyl and thiodicarb. This kind of pesticide is a good broad-spectrum insecticide. With the continuous growth of production, the market demand for acetaldoxime also increases. At the same time, acetaldehyde oxime is also an important organic synthesis reagent and analytical reagent. The acetaldehyde oxime...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/40C07C249/08C07C249/14
CPCC07C249/08C07C249/14C07C251/40
Inventor 叶茂伟刘建青汪俊杰李鲁祯
Owner 江苏艾科维科技股份有限公司
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