Purification method for methyl N-chloroformyl-N-[(4-trifluoromethoxy)phenyl]carbamate
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
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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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