Process for preparing 2-ethyl-N-(ethoxy methyl)-alpha-chloroacetanilide
A technology of ethoxymethyl and chloroacetyl, which is applied in the field of preparation of pesticide herbicides, can solve the problems of no record and no production of gramachlor, etc., and achieve the effects of less by-product pollutants, lower production costs, and high purity
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Embodiment 1
[0027] Step 1: Preparation of N-o-ethylphenyl-N-methyleneamine
[0028] Add 22g of o-ethylaniline (0.18mol) and 8.2g of paraformaldehyde (0.26mol) into a glass reactor with stirring and a thermometer, raise the temperature to 80°C, react for 2h, add 3.3g of ethanol when cooling to 60°C, and continue to heat up and reflux Reaction, steam 3.2g water, 3g ethanol, 1g formaldehyde mixture under negative pressure, add 50g xylene, get 23.2kg N-o-ethylphenyl-N-formimine (97% yield);
[0029] The second step: prepare 2-ethyl-phenyl-N-chloromethyl acetanilide intermediate with 23.2g N-o-ethylphenyl-N-formimine (0.174mol) and weigh 21.8g chloroacetyl chloride (0.187mol) was added to a glass reactor with stirring and a thermometer, the temperature was raised to 85°C and kept for 1h, and the solvent was evaporated to obtain 38g of 2-ethyl-phenyl-N-chloromethylacetanilide intermediate, with a yield of 88%;
[0030] The third step: preparation of crude oil of 2-ethyl-N-(ethoxymethyl)-α-chlo...
Embodiment 2
[0033] Step 1: Preparation of N-o-ethylphenyl-N-methyleneamine
[0034] Add 244kg of o-ethylaniline (2.0kmol) and 82.1kg of paraformaldehyde (2.6kmol) into the enamel reaction kettle with stirring and thermometer, heat up to 80°C, react for 2.5h, add 32kg of ethanol when cooling to 60°C, continue to heat up and reflux Reaction, steam 34% water, ethanol 30kg formaldehyde 22kg mixture under negative pressure, add 50kg xylene, get 254.8kg N-o-ethylphenyl-N-methylimine (96% yield);
[0035] The second step: preparation of 2-ethyl-phenyl-N-chloromethyl acetanilide intermediate
[0036] React 133g of N-o-ethylphenyl-N-methylimine (0.174mol) and 140g of chloroacetyl chloride at 100°C for 4h, distill off the solvent xylene to obtain the product 2-ethyl-phenyl-N-chloromethyl Acetanilide intermediate 244g, content 91%, yield 90%;
[0037] The third step: preparation of crude oil of 2-ethyl-N-(ethoxymethyl)-α-chloroacetylanilide
[0038] Put 50g of 2-ethyl-phenyl-N-chloromethyl acetan...
Embodiment 3
[0040] Add 21.2g of o-ethylaniline and 21.8g of chloroacetyl chloride into a glass reactor with stirring and a thermometer, raise the temperature to 80°C and keep it for 1 hour. After adding 4g of DMF, add 159g (1.73mol) of chloromethyl chloroformate dropwise. React at 90°C for 3.5 hours, then add the reactant to 310g ethanol to reflux for 0.5 hours, cool to 60°C, evaporate the ethanol and filter to remove a little sediment, the product 2-ethyl-N-(ethoxymethyl)-α-chloro Acetanilide 38g, yield 88%.
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