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Method for synthesizing 2-chloropropionaldehyde

A technology of chlorpropionaldehyde and chlorine gas, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, carbon-based compounds, etc., can solve the problems of high acidity of products, many drying operation steps, and overheating, and achieve product purity and High yield, mild reaction conditions, and the effect of avoiding water removal operation

Active Publication Date: 2015-01-07
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent US3240813 discloses a method for preparing 2-chloropropanal with hydrochloric acid system, but it has the following disadvantages: 1. the acidity requirement is very high in the reaction process, and the acidity of the system needs to be controlled at all times, otherwise the yield of the product will be seriously affected; 2. 2-chloropropanal Aldehyde and water are azeotropic, and the product drying operation steps are many and cumbersome during post-treatment, resulting in large product loss
[0004] Donald Craig has reported a kind of method that uses sulfuryl chloride to prepare 2-chloropropionaldehyde as chlorinating agent chlorinated propionaldehyde, but it has following deficiency: 1. the dropping temperature of sulfuryl chloride requires to be controlled below-10 ℃, but the The heat is violent, and there will be a runaway temperature when the dropwise addition is started, resulting in the generation of a large amount of impurities in the product; ②When sulfuryl chloride is used as a chlorinating agent for chlorination, it will produce waste gas containing hydrogen chloride and sulfur dioxide, and the amount of "three wastes" is large; ③After post-processing, the product The acidity is too high, which is not conducive to 2-chloropropanal as an intermediate for the next experiment

Method used

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  • Method for synthesizing 2-chloropropionaldehyde
  • Method for synthesizing 2-chloropropionaldehyde
  • Method for synthesizing 2-chloropropionaldehyde

Examples

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Effect test

Embodiment 1

[0025] Add 102g (1.2 moles) of dichloromethane and 5g (0.05 moles) of 36.5% hydrochloric acid into a 250mL four-neck flask equipped with a stirrer and a thermometer, keep away from light, control the temperature of the reaction system at 10-15°C, and then blow with nitrogen. Sweep the system for 10 minutes, then pass chlorine gas, the flow rate of chlorine gas is 17L / hr. After 10 minutes of chlorine gas flow, 58.1 g (1 mole) of propionaldehyde was added dropwise for a total of 2 hours. After the dropwise addition, chlorine gas was passed for 1 hour to react, then chlorine gas was stopped, and nitrogen gas was continued to purge excess chlorine gas in the system for 30 minutes. Get chlorinated solution. Distill the obtained chlorinated liquid under reduced pressure, and collect the distillate at 60-62°C / 185mmHg. The product has a purity of 99%, a yield of 92.4%, and a b.p. of 84-86°C.

Embodiment 2

[0027] Operation process is the same as embodiment 1, and catalyst is iron trichloride 8.1g (0.05 mol), makes chlorinated liquid, and the chlorinated liquid of gained is subjected to vacuum distillation, receives the cut of 60~62 ℃ / 185mmHg. Product yield 90.2%, b.p.84~86℃.

Embodiment 3

[0029] The operation process is the same as in Example 1, the reaction temperature is 50° C., and the chlorinated liquid is obtained, and the obtained chlorinated liquid is subjected to vacuum distillation, and the fraction of 60~62° C. / 185 mmHg is collected. Product yield 84.5%, b.p.84~86℃.

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Abstract

The invention relates to a chemical synthesis process and particularly relates to a method for synthesizing 2-chloropropionaldehyde. In the method, chloralkane is used as a solvent, acid is used as a catalyst, chlorine gas is used a chlorine source, propionaldehyde is used as a raw material, and the dosage of the acidic catalyst used in the invention is a catalytic dosage, so that the problem of high acidity of a product during after-treatment is solved; the reaction condition is mild, and no problems such as temperature runaway and the like exist; the reaction time is short; almost no water or a small deal of water is contained in a chlorination liquid, so that the complex dewatering operation during the after-treatment is avoided; and the product is high in purity and yield and few in three wastes.

Description

technical field [0001] The invention relates to a chemical synthesis process, in particular to a method for synthesizing 2-chloropropanal. Background technique [0002] 2-Chloropropanal is an important organic chemical raw material and an important organic intermediate for the synthesis of pesticides and medicines. [0003] Patent US3240813 discloses a method for preparing 2-chloropropanal with hydrochloric acid system, but it has the following disadvantages: 1. the acidity requirement is very high in the reaction process, and the acidity of the system needs to be controlled at all times, otherwise the yield of the product will be seriously affected; 2. 2-chloropropanal Aldehyde and water are azeotropic, and the drying operation steps of the product during post-treatment are many and cumbersome, and the product loss is large. [0004] Donald Craig has reported a kind of method that uses sulfuryl chloride to prepare 2-chloropropionaldehyde as chlorinating agent chlorinated p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/14C07C45/63
Inventor 顾克军丁克鸿徐林吴莎张晓谕阮禾
Owner JIANGSU YANGNONG CHEM GROUP
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