Purification method for methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate
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A technology of methyl carbamate and trifluoromethoxy, which is applied in the field of refining N-chloroformyl-N-[phenyl] methyl carbamate, and can solve the problems of low methyl carbamate content and the like
Inactive Publication Date: 2018-09-28
HUNAN GOFAR FINE CHEM IND TECH CO LDT
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But the N-chloroformyl [(4-trifluoromethoxy) phenyl] methyl carbamate product that this method produces contains unreacted N-[(4-trifluoromethoxy) phenyl] amino Methyl formate, resulting in low levels of methyl N-chloroformyl-N[(4-trifluoromethoxy)phenyl]carbamate in the product
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Embodiment 1
[0037] 100g of N-chloroformyl-N-[(4-trifluoromethoxy) phenyl] methyl carbamate product (N-chloroformyl-N-[(4-trifluoromethoxy) The mass content of phenyl] methyl carbamate is 92.5%), 212.5g of n-hexane and 37.5g of methyl acetate are mixed, stirred and heated to reflux state, dissolved for 2 hours, slowly cooled to -2°C~2°C, frozen and crystallized, Filter and dry to obtain 91.1g of refined product.
[0038] After testing, the mass content of methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate in the above-mentioned refined product was 96.5%, and the yield was 95%.
Embodiment 2
[0052] 100g of N-chloroformyl-N-[(4-trifluoromethoxy) phenyl] methyl carbamate product (N-chloroformyl-N-[(4-trifluoromethoxy) The mass content of phenyl] methyl carbamate is 92.5%), 225g of n-hexane and 25g of methyl acetate are mixed, stirred and heated to reflux state, dissolved for 2 hours, slowly cooled to -2°C~2°C, frozen and crystallized, filtered, After drying, 93g of refined product was obtained. The filtrate obtained by filtration was recovered and used mechanically.
[0053] After testing, the mass content of methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate in the above-mentioned refined product was 96%, and the yield was 96.5%.
Embodiment 3
[0055] 100g of N-chloroformyl-N-[(4-trifluoromethoxy) phenyl] methyl carbamate product (N-chloroformyl-N-[(4-trifluoromethoxy) The mass content of phenyl] methyl carbamate is 92.5%), 200g of n-hexane and 50g of methyl acetate are mixed, stirred and heated to reflux state, dissolved for 2 hours, slowly cooled to -2°C~2°C, frozen and crystallized, filtered, After drying, 86.8 g of refined product was obtained.
[0056] After testing, the mass content of methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate in the above-mentioned refined product was 97%, and the yield was 91%.
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Abstract
The invention provides a purification method for methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate. The purification method comprises the steps of: 1) providing a to-be-purified methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate product; 2) mixing the to-be-purified methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate product with n-hexane and methyl acetate, heating the mixture to reflux, dissolving the components for more than one hour to obtain a mixed liquid; 3) cooling the mixed liquid to -2 DEG C to 2 DEG C, performing freeze-crystallization, and filteringand drying the mixture to prepare the purified product. In the method, by means of difference of the solubility of the methyl N-[(4-trifluoromethoxy)phenyl]carbamate and the methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate in the n-hexane and methyl acetate, impurities can be effectively separated, and mass percentage of the methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate in the product is increased to more than 96%.
Description
technical field [0001] The invention relates to a method for refining acid chloride compounds, in particular to a method for refining methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate. Background technique [0002] Indoxacarb (indoxacarb) is a carbamate insecticide containing an oxadiazine structure developed by DuPont in the United States in 1992. The chemical name is (4aS)-7-chloro-2,3,4a,5- Tetrahydro-2{methoxycarbonyl[(4-trifluoromethoxy)phenyl]carbamoyl}indeno[1,2-e][1,3,4-]oxadiazine-4a-carboxy acid methyl ester. It is a chiral molecule, which is valued by the global pesticide industry because of its high efficiency, low toxicity, low residue, wide insecticidal spectrum and no carcinogenic, teratogenic and mutagenic effects. Its mechanism of action is to block the sodium ion channels in the nerve cells of pests, causing target pests to lose control, paralyze, unable to eat and finally die, thus protecting the target crops well. [0003] Methyl N-chlorofo...
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