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S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate as well as synthesis method and application of S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate

A technology of dihydroisoxazole and ethyl ethosulfate, which is applied in the production of organic chemistry and bulk chemicals, can solve the problems of great harm to the environment and human beings, difficult to treat wastewater, etc., and achieves low equipment requirements, fast reaction speed, The effect of high product purity

Active Publication Date: 2021-07-20
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above process route uses 5,5-dimethyl-4,5-dihydroisoxazolethiamidine hydrochloride as an intermediate, 1-methyl-3-(trifluoromethyl)-1H-pyrazole-5 A large amount of ammonia nitrogen waste water will be produced in the reaction process of -alcohol, formaldehyde aqueous solution and 5,5-dimethyl-4,5-dihydroisoxazole thiamidine hydrochloride. These waste water are difficult to treat and are very harmful to the environment and human beings.

Method used

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  • S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate as well as synthesis method and application of S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate
  • S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate as well as synthesis method and application of S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate
  • S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate as well as synthesis method and application of S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] At room temperature, 3-chloro-5-dimethyl-4,5-dihydroxazole (compound) shown in formula (I) was sequentially added in 60 ml of ethanol, and 12.1 g of potassium thioacetate. Then heated to 80 ° C stirring reaction, 4HR was used to detect no 3-chloro-5,5-dimethyl-4,5-dihydro isoxazole, the reaction was completed, and the reaction liquid was completed, and the inorganic salt was removed. After the filtration, the mother liquor was evaporated to evaporase, 17.7.7 g of the oil was 17.7 g, which is S- (5, 5-dimethyl-4,5-dihydrozole-3-yl) ethyl sulfate. . After HPLC detection, the purity of the product was 93%, and the yield was 95.1% in 3-chloro-5,5-dimethyl-4,5-dihydroxazole.

Embodiment 2

[0037]At room temperature, 3-chloro-5,5-dimethyl-4,5-dihydroxazole 13.3 g and potassium thioacetate were sequentially added in 60 ml of acetonitrile, and then heated to 75 ° C stirring reaction, 4HR The non-3-chloro-5,5-dimethyl-4,5-dihydroxazole was detected by HPLC, and the reaction was completed, the reaction solution was cooled to room temperature, and the inorganic salt was removed, and the filtered mother liquor was evaporated. Acetonitrile. After constant weight, 17.9 g of the oil was obtained, which was ethyl ester of S- (5,5-dimethyl-4,5-dihydrooxazole-3-yl). After HPLC detection, the purity of the product was 94%, and the yield was 97.3% in 3-chloro-5,5-dimethyl-4,5-dihydroxazole.

Embodiment 3

[0039] At room temperature, 3-chloro-5,5-dimethyl-4,5-dihydrozole 13.3 g and 12.7 g of thiococciocetate were sequentially added in 60 ml of methanol, and then heated to 65 ° C stirring reaction, 5HR No 3-chloro-5,5-dimethyl-4,5-dihydroxazole was detected with HPLC, and the reaction was completed, the reaction solution was cooled to room temperature, and the inorganic salt was removed, and the filtered mother liquor was evaporated. After constant weight, 17.2 g of the oil were obtained, which was S- (5,5-dimethyl-4,5-dihydrozole-3-yl) ethyl sulfate. After HPLC detection, the purity of the product was 94%, and the yield was 93.5% in 3-chloro-5,5-dimethyl-4,5-dihydroxazole.

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Abstract

The invention discloses S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate as well as a synthesis method and application of the S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate. According to the preparation method, 3-halogenated-5, 5-dimethyl-4, 5-dihydroisoxazole reacts with potassium thioacetate to prepare S-(5, 5-dimethyl-4, 5-dihydroisoxazole-3-yl) ethyl sulfate. According to the method, the synthesis process is simplified, the reaction speed is high, the product purity is high, the yield is high, the reaction condition is mild, the equipment cost is low, the synthesis process and the post-treatment process are extensive, the product is easy to separate, the obtained product can be used as a pyroxasulfone intermediate, and a plurality of defects of the 5, 5-dimethyl-4, 5-dihydroisoxazole thiamidine hydrochloride intermediate are avoided.

Description

Technical field [0001] The present invention relates to a S- (5-dimethyl-4, 5-dihydro isoxazole-3-yl) sulfate and its synthetic method, and also involves the S- (5, 5-) Application of methyl-4,5-dihydro isoxazole-3-yl) ethyl sulfate as an intermediate of sulfone pyrazole. Background technique [0002] Pyroxasulfone is an iszazole herbicide, developed by Japanese Combination Chemical Co., Ltd. is 3- [5- (Difluoromethoxy) -1-methyl-3- ( Trifluoromethyl) pyrazole-4-ylmethylsulfonyl] -4,5-dihydro-5,5-dimethyl-1,2-isoxazole, molecular formula C 12 Hide 14 Fly 5 N 3 O 4 S, the molecular weight is 391.32, and the CAS login number is 44,7399-55-5. Sulfonepotzole can be used in the pre-buds before the field of the field, after administration, the weed seedlings and young buds, inhibit the early growth of seedlings, destroying the biopsy and germ sheath, is a plant body VLCFA (extreme long side Severe potential inhibitors of chain fatty acids) (C20 ~ C30) biosynthesis. The structure is as ...

Claims

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Application Information

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IPC IPC(8): C07D261/04C07D413/12
CPCC07D261/04C07D413/12Y02P20/55
Inventor 王嵩宋健郝守志
Owner SHANDONG RUNBO BIOTECH CO LTD
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