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CAS No. : | 186204-66-0 | MDL No. : | MFCD01831028 |
Formula : | C8H5F2NO2S2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SHKGYNFSRWBSDZ-UHFFFAOYSA-N |
M.W : | 249.26 | Pubchem ID : | 3653678 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313 | UN#: | N/A |
Hazard Statements: | H315-H319 | Packing Group: | N/A |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83% | With hexaammonium heptamolybdate tetrahydrate; dihydrogen peroxide; In ethanol; at 20℃; for 42h; | A mixture of 7.18 g (33.05 mmol) of 2-[(difluoromethyl)sulfanyl]-1,3-benzothiazole, 2.04 g (1.65 mmol) of ammonium molybdate (NH4)6Mo7O24 x 4 H2O, 33.0 mL of ethanol, and 12.8 mL (132 mmol) of 30% H2O2 was stirred for 24 h at room temperature. An additional 3.5 mL of 30% H2O2 was added, the mixture was stirred for 18 h and diluted with 300 mL of water, and the precipitate was filtered off, washed with 500 mL of water, and dried at 120-130C. Yield 6.80 g (83%), white needles, mp 155-158C (from EtOAc); published data: mp 133-135C [11], 149C [12]. 1H NMR spectrum (CDCl3), δ, ppm: 6.60 t (1H, JHF = 53.1 Hz), 7.66 m (1H), 7.72 m (1H), 8.08 m (1H), 8.33 m (1H). 13C NMR spectrum (CDCl3), δC, ppm: 114.50 t (JCF = 288.1 Hz), 122.38, 126.25, 128.26, 129.07, 137.85, 153.01, 158.90. 19F NMR spectrum (CDCl3): δF -121.41 ppm. |
With sodium periodate; rhodium(III) chloride hydrate; In tetrachloromethane; water; acetonitrile; at 20℃; for 48h; | in a round bottom flask, add B in order.Acetonitrile,Carbon tetrachloride,Water and hydrated barium chloride.Place it on a stirrer and stir it vigorously.Then add 2.5 equivalents of sodium periodate to it,Finally let it continue to react at room temperature for 48 h.After treatment: saturated sodium bicarbonate solution and the reaction solution,filter,The filter residue was washed with ethyl acetate,The filtrate was extracted three times with ethyl acetate.After the organic phases are combined, they are dried over anhydrous magnesium sulfate.Spin-dry the solvent to give the desired product as a white solid. | |
With sodium periodate; ruthenium(III) chloride trihydrate; In tetrachloromethane; water; acetonitrile; at 25℃; for 0.5h;Inert atmosphere; | Step 2: To a solution of 2-((difluoromethyl)thio)benzo[rfjthiazole (11.1 g, 51 mmol) in a mixture of ACN / CC / water (v : v : v :::: 1 : 1 : 2, 222 mL) were added sodium periodate (34.2 g , 160 mmol) and ruthenium(III) chloride trihydrate (33 mg, 0.13 mmol) portion wise. The resulting solution was stirred at room temperature for 3 h. The mixture was diluted with water (800 ml) and extracted with DCM (1500 mL). The organic phase w?as washed with brine (800 mL), dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure, and the residue was purified by column chromatography on silica (0-20% ethyl acetate/DCM) to give 2-((difluoromethyl)suifonyl)benzo[ |
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