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A technology of chloroacetamide and synthesis method, which is applied to the preparation of organic compounds, chemical instruments and methods, preparation of carboxylic acid amides, etc. Equipment requirements, the effect of high product yield and high purity
Inactive Publication Date: 2019-08-13
WEIFANG SINO AGRI UNION CHEM CO LTD
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[0003] The current production process for synthesizing chloroacetamide compounds is complicated, and a large amount of hydrogen chloride gas will be generated during the reaction process. Generally, the reaction system needs to be kept in a negative pressure state, and the requirements for reaction conditions and production equipment are strict. In the current synthesis method, generally An acid-binding agent will be added, but this method will produce more salt and a small amount of alkali-containing wastewater. In order to remove the salt generated by the acid-binding agent during the post-treatment process after the reaction, a large amount of water is required for washing. This operation will also A large amount of salty wastewater is produced, the post-treatment process is difficult, and it does not meet the current national green environmental protection requirements
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Embodiment 1
[0044]
[0045] A kind of synthetic method of chloroacetamide compound, in reaction kettle, 107.16kg secondary amine compound A1 is dissolved in 53.58kg benzene, is warmed up to reflux, 112.94kg chloroacetyl chloride is added thereto, reflux reaction 0.5 hour, removes Solvent benzene, obtain 179kg chloroacetamide compound B1, productive rate is 97%, purity 98.4%; And reactor is connected with the water absorption device of hydrogen chloride gas, the hydrogen chloride gas produced in the reaction is absorbed by water absorption device, obtains industrial hydrochloric acid.
Embodiment 2
[0047]
[0048] A kind of synthetic method of chloroacetamide compound alachlor, in reaction kettle, 193.29kg secondary amine compound A2 is dissolved in 9664.5kg organic solvent toluene, is heated up to reflux, 338.82kg chloroacetyl chloride is added thereinto, reflux reaction 20 Hour, obtain 251kg chloroacetamide compound B2 (alachlor), productive rate is 93%, purity 98.2%; Reactor is connected with the water absorber of hydrogen chloride gas, and the hydrogen chloride gas produced in the reaction is absorbed by water absorber, Get industrial hydrochloric acid.
Embodiment 3
[0050]
[0051] A kind of synthetic method of chloroacetamide compound acetochlor, in reaction kettle, 193.29kg secondary amine compound A3 is dissolved in 386.58kg organic solvent sherwood oil, heat up to reflux, add 225.88kg chloroacetyl chloride wherein, reflux reaction 5 hours, add water 70kg and carry out washing, leave standstill for half an hour to separate liquid, organic phase removes solvent, obtains 246 chloroacetamide compounds B3 (acetochlor), productive rate is 91%, purity 98.1%; Reactor is connected with A water absorption device for hydrogen chloride gas, the hydrogen chloride gas generated in the reaction is absorbed by the ethanol aqueous solution with a mass concentration of 0.5% in the water absorption device to obtain industrial hydrochloric acid.
[0052] Inside the water absorption device is; the temperature inside the water absorption device is 0-20°C
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Abstract
The invention discloses a synthesizing method for a chloroacetamide compound. In a reaction kettle, a secondary amine compound is dissolved in an organic solvent, the mixture is heated for reflux, chloroacetyl chloride is added into the mixture, a reflux reaction is conducted for 0.5-20 hours, and the chloroacetamide compound is obtained. According to the synthesizing method for the chloroacetamide compound, an acid binding agent is not used, discharging of wastewater in the after-treatment process is reduced, by keeping the reflux state of the system, hydrogen chloride gas generated from thereaction is exhausted out of the system and absorbed by water outside the system, high-purity hydrochloric acid is obtained, the waste is turned into wealth, the method comes up to the production standard of safety and environment protection, and discharging of waste gas, waste water and waste residues is reduced; according to the synthesizing method for the chloroacetamide compound, few operationsteps are utilized, the reaction speed is high, the product yield is high, the purity is high, the production cost is low, and the method is safe, friendly to the environment and suitable for industrial large-scale production.
Description
technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing chloroacetamide compounds. Background technique [0002] Chloroacetamide compounds are a class of important organic compounds, alachlor, acetochlor, pretilachlor, propachlor, butachlor, metazachlor, metacetamine, dimethachlor ( High-efficiency metolachlor), metolachlor and refined metolachlor are all outstanding representatives of this class of compounds, and refined metolachlor is one of the best. The refined metolachlor was developed by Syngenta, and it went on the market in the United States in 1997. On October 16, 2001, the protection period of the US patent expired. Metolachlor, like metolachlor, is a cell division inhibitor, but according to the results of toxicology studies, its toxicity is lower than that of metolachlor, only one-tenth of the toxicity of the latter. Slim metolachlor has a wide crop spectrum and is the main herbicide u...
Claims
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