Method for producing 2-methyl-4-MCPA
A technology of methylphenoxyacetic acid and chlorophenoxyacetic acid is applied in chemical instruments and methods, preparation of carboxylates, preparation of organic compounds, etc., and can solve problems such as low product purity, increased environmental pollution, and increased cost. , to achieve the effect of high yield, obvious environmental protection advantages, and realization of production costs
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Embodiment 1
[0020] Add 2-methylphenoxyacetic acid 41g (content 98%, 0.242mol), dimethylaminopyridine 0.5g (content 99%), dimethylformamide 2.5g (content 99%) and 8% 363 g (0.726 mol) of sodium hydroxide aqueous solution was stirred and dissolved at room temperature. Maintain the reaction temperature at 20-25°C, feed about 28g of chlorine gas into the material at a rate of 5-10kg / hr, and when the content of 2-methylphenoxyacetic acid in the raw material is less than 1% as monitored by HPLC, the reaction ends. During the process of passing chlorine, 2-methyl-4-chlorophenoxyacetic acid solids were continuously precipitated. Add concentrated hydrochloric acid dropwise to adjust the pH of the material to 1-2, lower the temperature to 0-5°C, filter, and dry the filter cake to obtain 47.6g of 2-methyl-4-chlorophenoxyacetic acid as a white solid, the active ingredient being 2-methyl The content of base-4-chlorophenoxyacetic acid is 97.4%, and the yield is 95.5%.
Embodiment 2
[0022] A method for producing 2-methyl-4-chlorophenoxyacetic acid, 2-methylphenoxyacetic acid is dissolved in aqueous sodium hydroxide solution, catalyst dimethylaminopyridine and dimethylformamide are added, and chlorine gas is introduced to react After the reaction is completed, the temperature is lowered to crystallize, and then separated by filtration and dried to obtain the finished product 2-methyl-4-chlorophenoxyacetic acid.
[0023] The mass ratio of 2-methylphenoxyacetic acid and compound solvent is 1: 1~100 (example 1: 1, 1: 50, 1: 100); The mass ratio of catalyst dimethylaminopyridine and dimethylformamide is 1:1~10 (example 1:1, 1:5, 1:10); the mass ratio of the total mass of catalyst dimethylaminopyridine and dimethylformamide to 2-methylphenoxyacetic acid is 1:50~ 800 (example 1: 50, 1: 400, 1: 800); the reaction temperature of feeding chlorine gas is 10-100 °C (example 10 ° C, 50 ° C, 100 ° C); 2-methylphenoxyacetic acid and the feeding of chlorine gas The mola...
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