A kind of synthesis technology of fenoxuron
A synthesis process and a technology for decoxolone are applied in the field of synthesis process of decopaxone, which can solve problems such as increasing environmental protection pressure and capital investment, and achieve the effects of easy industrial production, simple operation, and lower production costs.
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Embodiment 1
[0038] A kind of synthetic technique of oxazone, comprising the following steps:
[0039] Add 1.49kg of 3,4-dihydro-3-methyl-2H-1,4-benzoxazine and 4.47kg of solvent cyclohexane into the reaction kettle, stir and dissolve, connect the reaction kettle to the tail gas absorption device, heat up to reflux 1.47kg of dichloroacetyl chloride was added dropwise, and the dropwise addition time was 1 hour. After the dropwise addition, the reflux reaction was carried out for 1 hour to obtain the reaction solution;
[0040] The resulting reaction solution was distilled under reduced pressure, and the solvent was removed to obtain 2.55 kg of crude product, with a content of 95.2%, and a yield of 98.1%. The resulting crude product was recrystallized with 5.1 kg of methanol to obtain 2.50 kg of oxalum, with a content of more than 99.0%, and a yield of 96.2 %.
[0041] The solvent cyclohexane in this embodiment is also replaced with n-hexane, methylene dichloride, ethylene dichloride, chlor...
Embodiment 2
[0043] A kind of synthetic technique of oxazone, comprising the following steps:
[0044] Add 1.49kg of 3,4-dihydro-3-methyl-2H-1,4-benzoxazine and 14.9kg of dichloromethane into the reaction kettle, stir and dissolve, connect the reaction kettle to an exhaust gas absorption device, raise the temperature to reflux and then add dropwise 2.20kg of dichloroacetyl chloride, reflux reaction for 3 hours after the dropwise addition, to obtain a reaction solution; the time for dropping dichloroacetyl chloride is limited to 3 hours;
[0045] The resulting reaction solution was distilled under reduced pressure, and the solvent was removed to obtain 2.56 kg of crude product, with a content of 95.4%, and a yield of 98.5%. The resulting crude product was recrystallized with 10.24 kg of methanol to obtain 2.49 kg of oxalum, with a content of more than 99.0%, and a yield of 95.8 %.
[0046] The solvent dichloromethane in this embodiment is also replaced with normal hexane, cyclohexane, ethy...
Embodiment 3
[0048] A kind of synthetic technique of oxazone, comprising the following steps:
[0049] Add 1.49kg of 3,4-dihydro-3-methyl-2H-1,4-benzoxazine and 5.96kg of toluene into the reaction kettle, stir and dissolve, connect the reaction kettle to the tail gas absorption device, raise the temperature to reflux and add 1.76kg dropwise kg of dichloroacetyl chloride, reflux reaction for 2.5 hours after the dropwise addition, to obtain a reaction solution; the time for dripping dichloroacetyl chloride was limited to 2 hours;
[0050] The resulting reaction solution was distilled under reduced pressure, and the solvent was removed to obtain 2.55 kg of crude product, with a content of 95.6%, and a yield of 98.2%. The resulting crude product was recrystallized with 7.66 kg of methanol to obtain 2.48 kg of oxalum, with a content of more than 99.0%, and a yield of 95.4 %.
[0051] The solvent toluene in this embodiment is also replaced with n-hexane, methylene dichloride, ethylene dichlorid...
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