Preparation method of chlorantraniliprole
A technology of chlorantraniliprole and methanol, which is applied in the field of preparation of chlorantraniliprole, can solve the problems that the production process is not easy to control, is not suitable for industrial production, and harsh reaction conditions, so as to achieve suitable industrial development and easy industrialization The effect of easy production and post-processing
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Embodiment 1
[0029] The invention provides the following technical scheme: a preparation method of chlorantraniliprole, comprising the following steps:
[0030] 1) Add 4 parts of maleic anhydride and 4 parts of methanol into a single-necked bottle, stir and raise the temperature to 50°C and keep it warm for 0.5h to prepare monomethyl maleate;
[0031] 2) Cool 80 parts of hydrogen bromide-glacial acetic acid solution to 0°C, then dropwise add 3 parts of monomethyl maleate, keep stirring after adding, a large amount of yellow viscous substance will appear after 3 minutes, and 3-bromomaleic acid can be obtained monomethyl ester;
[0032] 3) Dissolve monomethyl 3-bromomaleate in 10 parts of dichloromethane, then add 4 drops of DMF dropwise, and add 2 parts of thionyl chloride dissolved in dichloromethane solution dropwise within 10 minutes to obtain 3-bromo Monomethyl maleate chloride;
[0033] 4) Add 18 parts of 2,3-dichloropyridine and 26 parts of ethylene glycol into a single-necked bottl...
Embodiment 2
[0042] The invention provides the following technical scheme: a preparation method of chlorantraniliprole, comprising the following steps:
[0043] 1) Add 6 parts of maleic anhydride and 6 parts of methanol into a single-neck bottle, stir and raise the temperature to 50°C and keep it warm for 1 hour to prepare monomethyl maleate;
[0044] 2) Cool down 100 parts of hydrogen bromide-glacial acetic acid solution to 0°C, add 4 parts of monomethyl maleate dropwise, keep stirring after adding, a large amount of yellow viscous substance will appear after 3-7 minutes, and 3-bromomaleic acid can be obtained. monomethyl torate;
[0045] 3) Dissolve 3-bromomonomethyl maleate in 13 parts of dichloromethane, then add 5 drops of DMF dropwise, and add 3 parts of thionyl chloride dissolved in dichloromethane solution dropwise within 15 minutes to obtain 3-bromo Monomethyl maleate chloride;
[0046] 4) Add 21 parts of 2,3-dichloropyridine and 28 parts of ethylene glycol into a single-necked ...
Embodiment 3
[0055] The invention provides the following technical scheme: a preparation method of chlorantraniliprole, comprising the following steps:
[0056] 1) Add 8 parts of maleic anhydride and 8 parts of methanol into a single-necked bottle, stir and raise the temperature to 50°C and keep it warm for 1.5h to prepare monomethyl maleate;
[0057] 2) Cool 120 parts of hydrogen bromide-glacial acetic acid solution to 0°C, add 5 parts of monomethyl maleate dropwise, keep stirring after adding, a large amount of yellow viscous substance will appear after 7 minutes, and 3-bromomaleic acid can be obtained monomethyl ester;
[0058] 3) Dissolve 3-bromomonomethyl maleate in 15 parts of dichloromethane, then add 6 drops of DMF dropwise, and add 4 parts of thionyl chloride dissolved in dichloromethane solution dropwise within 20 minutes to obtain 3-bromo Monomethyl maleate chloride;
[0059] 4) Add 24 parts of 2,3-dichloropyridine and 30 parts of ethylene glycol into a single-necked bottle to...
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