Production method of methyl o-formate benzyl sulfonamide

A technology of methyl benzyl sulfonamide and acid methyl benzyl sulfonyl chloride is applied in the field of production of methyl o-formate benzyl sulfonamide, which can solve the problems of high cost and low yield, reduce production, increase The effect on product yield

Active Publication Date: 2020-09-01
淄博腾煜化工工程有限公司
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  • Summary
  • 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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  • Production method of methyl o-formate benzyl sulfonamide
  • Production method of methyl o-formate benzyl sulfonamide

Examples

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Embodiment 1

[0045] (1) Synthetic of o-chloromethylbenzoic acid: add solvent dichloroethane 500kg in reactor, add o-toluic acid 300kg again, and catalyst azobisisobutyronitrile 4kg, steam is warming up to 60 ℃ of refluxes, Add 350kg of the chlorinating agent sulfuryl chloride dropwise, carry out reflux reaction, react for 4 hours, and synthesize o-chloromethylbenzoic acid under catalysis; after the reaction is finished, distill and recover the solvent, then add clear water to stir and cool down to crystallize, filter and dry to obtain o-chloromethylbenzoic acid Benzoic acid crystal 368kg, content 97%, yield 98%;

[0046] (2) Synthetic of methyl o-chloromethylbenzoate: 368kg of o-chloromethylbenzoic acid synthesized by step (1) is added in the esterification reactor, then add 400kg methyl alcohol, add the concentrated sulfuric acid 150kg under stirring to be catalyzer, steam Heating to 80°C for esterification reaction, after 6 hours of reaction, distilling and recovering unreacted methanol,...

Embodiment 2

[0052] (1) Synthetic of o-chloromethylbenzoic acid: add solvent dichloroethane 500kg in reactor, add o-toluic acid 300kg again, and catalyst azobisisobutyronitrile 4kg, steam is warming up to 70 ℃ of refluxes, Add 360 kg of chlorinating agent sulfuryl chloride dropwise, carry out reflux reaction, react for 4 hours, and synthesize o-chloromethylbenzoic acid under catalysis; after the reaction is completed, distill and recover the solvent, then add clear water to stir and cool down to crystallize, filter and dry to obtain o-chloromethylbenzoic acid Benzoic acid crystal 365kg, content 98%, yield 97%;

[0053] (2) Synthetic of methyl o-chloromethylbenzoate: 365kg of o-chloromethylbenzoic acid synthesized by step (1) is added in the esterification reactor, then add 400kg methyl alcohol, add the concentrated sulfuric acid 150kg under stirring to be catalyzer, steam Heating to 60°C for esterification reaction, the reaction is over for 6 hours, distillation and recovery of unreacted m...

Embodiment 3

[0059] (1) Synthetic of o-chloromethylbenzoic acid: add solvent dichloroethane 500kg in reactor, add o-toluic acid 300kg again, and catalyst azobisisobutyronitrile 4kg, steam is warming up to 60 ℃ of refluxes, Add 365 kg of chlorinating agent sulfuryl chloride dropwise, carry out reflux reaction, react for 4 hours, and synthesize o-chloromethylbenzoic acid under catalysis; after the reaction is completed, distill and recover the solvent, then add clear water to stir and cool down to crystallize, filter and dry to obtain o-chloromethylbenzoic acid Benzoic acid crystal 368kg, content 97%, yield 98%;

[0060] (2) Synthetic of methyl o-chloromethylbenzoate: 368kg of o-chloromethylbenzoic acid synthesized by step (1) is added in the esterification reactor, then add 400kg methyl alcohol, add the concentrated sulfuric acid 150kg under stirring to be catalyzer, steam Heating to 100°C for esterification reaction, the reaction is over for 6 hours, distillation and recovery of unreacted ...

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Abstract

The invention belongs to the technical field of pesticide intermediates, and particularly relates to a production method of methyl o-formate benzyl sulfonamide. The production method comprises steps:reacting o-methylbenzoic acid with sulfuryl chloride to obtain o-chloromethylbenzoic acid; reacting o-chloromethylbenzoic acid with methanol to obtain o-chloromethyl methyl benzoate; reacting o-chloromethyl methyl benzoate with sodium thiosulfate to obtain methyl o-formate benzyl mercaptan, reacting methyl o-formate benzyl mercaptan with chlorine to obtain methyl o-formate benzyl sulfonyl chloride, and reacting methyl o-formate benzyl sulfonyl chloride with ammonia gas to obtain methyl o-formate benzyl sulfonamide. According to the method, polychlorinated side reactions in the production process are reduced, the yield is increased, the tar yield is reduced, and the problems of low yield and high cost in the production process are solved.

Description

technical field [0001] The invention belongs to the technical field of pesticide intermediates, in particular to a production method of methyl o-formate benzylsulfonamide. Background technique [0002] Bensulfuron-methyl (Nongdeshi, Daowucao, Biannong) was first used to control sedges and broad-leaved weeds in rice 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 of weeds by roots and leaves. It is safe for wheat, rice and other crops. Used in wheat fields, it can effectively control broad-leaved weeds such as pig's weeds, chickweed, rice shepherds, wormwood, shepherd's purse, succulents, quinoa, rice chaste, etc., usually in the 2-3 leaf stage of weeds, soil Spray with 30-40 grams of 10% bensulfuron-methyl per mu and add water when it is wet. The active ingredient of the drug diffuses rapidly in water, and the temperature and soil quality have l...

Claims

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Application Information

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Patent Type & Authority Applications(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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