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Preparation method for 3-chloropropionylchloride

A technology for chloropropionyl chloride and acrylic acid, which is applied in the preparation of acyl halide, the preparation of organic compounds, the preparation of carboxylate, etc., can solve the problems of high risk, complicated preparation method of 3-chloropropionyl chloride, etc., and achieves less post-processing steps. , The effect of high product yield and cost reduction

Active Publication Date: 2014-05-28
常州市正锋光电新材料有限公司
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Problems solved by technology

[0003] The present invention overcomes the disadvantages of complex and dangerous preparation methods of 3-chloropropionyl chloride in the prior art, and provides a preparation method of 3-chloropropionyl chloride

Method used

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  • Preparation method for 3-chloropropionylchloride
  • Preparation method for 3-chloropropionylchloride

Examples

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Embodiment

[0011] Add 200g of acrylic acid and 2g of water into a four-neck flask equipped with a stirrer, a thermometer and a condenser, add 360g of thionyl chloride dropwise below 20°C, slowly heat and reflux for 6 hours after dropping, and then distill at atmospheric pressure to 120°C. Distilled under reduced pressure to obtain 303g product again, yield 86%, content 99.1%. From figure 1 and figure 2 It can be confirmed that the final product obtained in this example is 3-chloropropionyl chloride.

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Abstract

A technical solution adopted by the invention relates to a preparation method for 3-chloropropionylchloride. The preparation method comprises the following steps of mixing acrylic acid and water; dropwise adding thionyl chloride at a temperature of 20 DEG C; refluxing for 3-8 h by heating until acrylic acid is reacted completely; distilling to a temperature of 120 DEG C under a normal pressure; and then distilling out a product under a reduced pressure. The preparation method has the beneficial effects that cost is greatly reduced than that of a two-step method; post treatment steps are few; and the product is high in yield and high in purity. Besides, according to the preparation method, water is added, thereby facilitating the reaction. Compared with preparation methods reported in the prior art, the preparation method has essential difference. Results of gas phase analysis and standard sample contrast analysis show that the product is 3-chloropropionylchloride. The product is used for preparing 3'-chloropropiophenone; and the product and the yield are the same.

Description

technical field [0001] The invention belongs to the field of chemical preparation, in particular to a preparation method of 3-chloropropionyl chloride. Background technique [0002] At present, there are mainly two methods for the relatively mature synthesis of 3-chloropropionyl chloride: ① direct method, acrylic acid and phosgene react to directly synthesize, this method makes a method suitable for large-scale industrial production; ② two-step method, first Synthesis of 3-chloropropionic acid followed by acyl chloride with thionyl chloride. The first method uses phosgene, which is costly and dangerous, and is not suitable for small enterprises; the 3-chloropropionic acid prepared in the first step of the two-step method is difficult to separate and the equipment is complicated. And because 3-chloropropionyl chloride reacts with water, it is strictly required to avoid the mixing of water in the reaction process, so as to avoid the generation of side reactions. Contents of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/50C07C51/60
CPCC07C51/58C07C53/50
Inventor 徐小虎
Owner 常州市正锋光电新材料有限公司
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