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The preparation method of diclosulam

A technology of diclofenac and chlorosulfonyl, applied in the field of preparation of diclofenac, can solve the problems of complicated operation, difficult control, low safety and the like, and achieves simple process conditions, simple operation and high safety. Effect

Active Publication Date: 2019-02-19
江苏省农用激素工程技术研究中心有限公司 +1
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Problems solved by technology

[0004] The disadvantage of this method is that the preparation of N-arylsulfimide catalyst requires the use of flammable, volatile, highly toxic, and malodorous dimethyl sulfide and the need to feed chlorine gas, which is not only complicated to operate, difficult to control, and low in safety , and the process conditions are harsh, the requirements for production equipment are high, and it is difficult to carry out industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0015] The preparation method of the diclosulam of the present embodiment is as follows:

[0016] Add 3,5-lutidine (32.1g, 0.30mol) into 85g of acetonitrile, stir to dissolve and add 2-chlorosulfonyl-7-fluoro-5-ethoxy[1,2,4]tri Azolo[1,5-c]pyrimidine (28.0g, 0.10mol) and 2,6-dichloroaniline (24.3g, 0.15mol), after stirring for 30min, add 0.3g of dimethyl sulfoxide, and finally stir to raise the temperature Reaction at 48°C for 24h.

[0017] After the reaction was completed, concentrated hydrochloric acid and water were added, stirred for 1 hour, and filtered with suction. The filter cake was washed with water, dried, and filtered with suction to obtain 37.4 g of diclosulam with a yield of 92.1% and a purity of 98.5% (HPLC).

Embodiment 2～ Embodiment 8）

[0019] The preparation method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.

[0020] Table 1

[0021]

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PUM

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Abstract

The invention discloses a preparation method of diclosulam. The diclosulam is prepared from 2-(chlorosulfonyl)-7-fluoro-5-ethoxy[1,2,4]triazolo[1,5-c]pyrimidine and 2,6-dichloroaniline through a condensation reaction in an organic solvent, wherein the condensation reaction is performed under catalysis of 3,5-dimetylpyridine; the mole ratio of 2-(chlorosulfonyl)-7-fluoro-5-ethoxy[1,2,4]triazolo[1,5-c]pyrimidine to 2,6-dichloroaniline is 1:1-1:5; the organic solvent is a mixed solvent containing DMSO (dimethyl sulfoxide), and the weight percentage of DMSO in the mixed solvent is 0.1%-1%. The method is higher in safety and simple and convenient to operate, process conditions are simple, higher reaction yield and product purity can be obtained by selecting a proper catalyst and a proper organic solvent, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of herbicide preparation, and in particular relates to a preparation method of diclosulam. Background technique [0002] Diclosulam is a triazolopyrimidine sulfonamide herbicide developed by Dow Agricultural Sciences Corporation of the United States. The CAS registration number is 145701-21-9. Chlorophenyl)-5-ethoxy-7-fluoro[1,2,4]triazolo[1,5-c]pyrimidine-2-sulfonamide. Diclosulam is mainly used for pre-emergence and pre-planting soil treatment of soybeans and peanuts to control broad-leaved weeds. The safety of soybeans and peanuts is based on its rapid metabolism and the formation of inactive compounds. [0003] Chinese patent document CN1216040A discloses a preparation method of diclosulam, which is catalyzed by a self-made N-aryl sulfimide compound, from 2-chlorosulfonyl-7-fluoro-5-ethoxy [1,2,4] Triazolo [1,5-c] pyrimidine and 2,6-dichloroaniline obtained by condensation reaction. [0004] The disad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 孙永辉张元元孔繁蕾史跃平高建红万里红
Owner 江苏省农用激素工程技术研究中心有限公司
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