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Method for preparing 6-fluoro-2-pyridinesulfonyl chloride

A technology of pyridinesulfonyl chloride and difluoropyridine difluoropyridine is applied in the field of preparing 6-fluoro-2-pyridinesulfonyl chloride, which can solve the problems of potential safety hazards, use safety risks, high toxicity and the like, and achieves improved safety and reliability. The effect of operability, reduction of raw material cost and production cost

Pending Publication Date: 2019-05-07
成都博腾药业有限公司
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] The shortcomings of this preparation method are: the use of extremely smelly and toxic benzyl mercaptan, the use of sodium hydride and chlorine gas with high safety risks, there are potential safety hazards

Method used

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  • Method for preparing 6-fluoro-2-pyridinesulfonyl chloride
  • Method for preparing 6-fluoro-2-pyridinesulfonyl chloride
  • Method for preparing 6-fluoro-2-pyridinesulfonyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Embodiment 1 (preparation of formula II)

[0013] Add 100g of water, 20g of sodium sulfide, and 8.2g of sulfur powder into the reaction flask, and heat the reaction until the sulfur powder dissolves to obtain an orange sodium disulfide solution. After cooling to room temperature, add 19.6 g of 2,6-difluoropyridine and ethanol to the reaction flask, heat the reaction until the raw materials disappear, add tertiary methyl ether for extraction after cooling, dry over anhydrous sodium sulfate, filter, and concentrate to obtain a yellow oil. The yield was 70%, and the purity of the product detected by HPLC was 92.2%.

Embodiment 2

[0014] Embodiment 2 (preparation of formula II)

[0015] Add 60g of water, 11.2g of sodium hydrosulfide, 50g of methanol, 4g of 2,6-difluoropyridine into the reaction flask, heat the reaction until the raw materials disappear, add tertiary methyl ether after cooling for extraction, dry over anhydrous sodium sulfate, filter, concentrate, A yellow oil was obtained with a yield of 52%, and the purity of the product detected by HPLC was 85.7%.

Embodiment 3

[0016] Embodiment 3 (preparation of formula II)

[0017] Add 150g of water, 23g of sodium sulfide, 60g of N,N-dimethylformamide, 5g of 2,6-difluoropyridine into the reaction flask, heat the reaction until the raw materials disappear, add tertiary methyl ether for extraction after cooling, anhydrous sodium sulfate Drying, filtration, and concentration gave a yellow oil with a yield of 33%. The purity of the product was 94.2% by HPLC.

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Abstract

The invention discloses a method for preparing 6-fluoro-2-pyridinesulfonyl chloride. 2,6-difluoropyridine is used as a starting material, through sulfurization of a substance of an inorganic sulfide compound of Na2S, NaHS, Na2Sx or the like, a persulfide (as shown in the formula II) is produced, and then the compound as shown in the formula II is subjected to oxidation to obtain the 6-fluoro-2-pyridinesulfonyl chloride.

Description

technical field [0001] field of medical technology. Background technique [0002] Documents US2009197859, US4987141, US5137886, WO201195576, US2011195979, US201695858, Bioorganic and Medicinal Chemistry, 2017, p. 3447-3460, etc. report the preparation method of 6-fluoro-2-pyridinesulfonyl chloride, see the following formula. These preparation methods have one thing in common, that is, 2,6-difluoropyridine is used as a raw material, and benzylthiol undergoes a nucleophilic substitution reaction under strong alkali conditions to obtain a thioether, which is then oxidized with chlorine or other oxidizing agents. produce the target product. [0003] [0004] The shortcomings of this preparation method are: the use of extremely smelly and highly toxic benzyl mercaptan, and the use of sodium hydride and chlorine gas with high safety risks, which have potential safety hazards. Contents of the invention [0005] Aiming at the defects of the prior art, the present invention di...

Claims

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Application Information

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IPC IPC(8): C07D213/71
Inventor 林文清郑宏杰刘小波
Owner 成都博腾药业有限公司
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