The production method of methyl o-formate benzylsulfonamide

A technology of methyl benzyl sulfonamide and methyl benzyl sulfonyl chloride, which is applied in the field of pesticide intermediates, can solve the problems of high cost and low yield, and achieve the effect of reducing production and increasing product yield

Active Publication Date: 2022-07-08
淄博腾煜化工工程有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of this invention is to provide a kind of production method of methyl o-formate benzyl sulfonamide, which reduces the side reaction of polychlorination in the production process, improves the yield, reduces the production amount of tar, and solves the problem of yield in the production process. The problem of low rate and high cost

Method used

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  • The production method of methyl o-formate benzylsulfonamide
  • The production method of methyl o-formate benzylsulfonamide

Examples

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Embodiment 1

[0045] (1) the synthesis of o-chloromethyl benzoic acid: in reactor, add solvent dichloroethane 500kg, then add o-toluic acid 300kg, and catalyzer azobisisobutyronitrile 4kg, steam is warming up to 60 ℃ of refluxes, Add chlorinating agent sulfuryl chloride 350kg dropwise, carry out reflux reaction, react for 4 hours, and synthesize o-chloromethyl benzoic acid under catalysis; After the reaction, the solvent is recovered by distillation, then add clear water and stir to cool down for crystallization, and filter and dry to obtain o-chloromethyl benzoic acid. 368kg of benzoic acid crystals, content 97%, yield 98%;

[0046] (2) synthesis of methyl o-chloromethyl benzoate: 368kg of o-chloromethyl benzoic acid synthesized by step (1) is added in the esterification reactor, then 400kg of methanol is added, and 150kg of vitriol oil is added under stirring to be a catalyzer, steam Heating to 80°C to carry out esterification reaction, the reaction was completed for 6 hours, the unreacte...

Embodiment 2

[0052] (1) synthesis of o-chloromethyl benzoic acid: in reactor, add solvent dichloroethane 500kg, then add o-toluic acid 300kg, and catalyzer azobisisobutyronitrile 4kg, steam is warming up to 70 ℃ of backflow, Add chlorinating agent sulfuryl chloride 360kg dropwise, carry out reflux reaction, react for 4 hours, and synthesize o-chloromethyl benzoic acid under catalysis; After the reaction, the solvent is recovered by distillation, then clear water is added, stirring is lowered, and temperature crystallization is performed, and o-chloromethyl benzoic acid is obtained by filtration and drying. 365kg of benzoic acid crystals, content 98%, yield 97%;

[0053] (2) synthesis of methyl o-chloromethyl benzoate: 365kg of o-chloromethyl benzoic acid synthesized by step (1) is added in the esterification reactor, then 400kg of methanol is added, and 150kg of vitriol oil is added under stirring to be a catalyst, steam Heating to 60° C. to carry out esterification reaction, the reaction ...

Embodiment 3

[0059] (1) the synthesis of o-chloromethyl benzoic acid: in reactor, add solvent dichloroethane 500kg, then add o-toluic acid 300kg, and catalyzer azobisisobutyronitrile 4kg, steam is warming up to 60 ℃ of refluxes, Add 365 kg of chlorinating agent sulfonyl chloride dropwise, carry out reflux reaction, react for 4 hours, and synthesize o-chloromethyl benzoic acid under catalysis; after the reaction, the solvent is recovered by distillation, then add clear water and stir to lower temperature for crystallization, and filter and dry to obtain o-chloromethyl benzoic acid. 368kg of benzoic acid crystals, content 97%, yield 98%;

[0060] (2) synthesis of methyl o-chloromethyl benzoate: 368kg of o-chloromethyl benzoic acid synthesized by step (1) is added in the esterification reactor, then 400kg of methanol is added, and 150kg of vitriol oil is added under stirring to be a catalyzer, steam Heating to 100°C to carry out esterification reaction, the reaction was over for 6 hours, the ...

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Abstract

The invention belongs to the technical field of pesticide intermediates, and in particular relates to a production method of methyl o-formate benzylsulfonamide. o-Toluic acid reacts with sulfuryl chloride to obtain o-chloromethyl benzoic acid, o-chloromethyl benzoic acid reacts with methanol to obtain methyl o-chloromethyl benzoate, and methyl o-chloromethyl benzoate reacts with sodium thiosulfate Obtain methyl o-formate benzyl mercaptan, methyl o-formate benzyl mercaptan reacts with chlorine to obtain methyl o-formate benzyl sulfonyl chloride, and methyl o-formate benzyl sulfonyl chloride reacts with ammonia to obtain methyl o-formate benzyl sulfonamide . The invention reduces the side reaction of polychlorination in the production process, improves the yield, reduces the amount of tar produced, and solves the problems of low yield and high cost in the production process.

Description

technical field [0001] The invention belongs to the technical field of pesticide intermediates, and in particular relates to a production method of methyl o-formate benzylsulfonamide. Background technique [0002] Bensulfuron-methyl (Nongdeshi, rice without grass, convenient farming) was first used to control sedge and broad-leaved weeds in paddy fields, and has been used to control broad-leaved weeds in wheat fields. Bensulfuron-methyl is a selective systemic herbicide, which is absorbed and transferred to various parts by weed roots and leaves, and has good safety on crops such as wheat and rice. Used in wheat fields, it can effectively control broad-leaved weeds such as pig's scourge, chickweed, broken rice chestnut, solanum vulgaris, shepherd's purse, large nest vegetable, quinoa, rice chakra, etc., usually at the 2-3 leaf stage of weeds, soil When wet, spray with 30-40 grams of 10% bensulfuron-methyl plus water per acre. The active ingredient of the medicine diffuses ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/38C07C311/13C07C303/02C07C309/84C07C319/02C07C323/56C07C67/08C07C69/78C07C51/363C07C63/70
CPCC07C303/38C07C303/02C07C319/02C07C67/08C07C51/363C07C63/70C07C69/78C07C323/56C07C309/84C07C311/13
Inventor 邓秋渠鲍兴亮韩婧刘淼
Owner 淄博腾煜化工工程有限公司
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