Method for electrochemical synthesis of alkyl sulfone compounds
A synthesis method and technology of alkyl sulfone, which is applied in the application field of alkyl sulfone compounds, can solve the problems of few reports, and achieve the effects of high atom economy, good inhibitory activity, and good functional group tolerance
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[0023] Example 1:
[0024] 9- (phenylsulfonyl) -9 H - xanthene (3 aa) Synthesis and Characterization:
[0025]
[0026] Respectively, 0.6 mmol benzenesulfonyl hydrazide, 0.3 mmol 9 H - xanthene, 0.06 mmol ammonium iodide and 0.6 mmol of potassium carbonate was added to 25 mL three-neck flask, was added 6 mL 1,2- dichloroethane and hexafluoroisopropanol mixture (v: v = 4: 2) dissolving, with the carbon rod as the anode, the platinum plate as the cathode, the reaction mixture was stirred for 3 hours at a constant current of 10 mA at normal temperature, TLC monitoring of the reaction progress;
[0027] After completion of the reaction, the mixture was extracted with ethyl acetate (10 mL). The organic layer was dried over anhydrous Na 2 SO 4 Drying, rotary evaporation under reduced pressure, and (silica gel eluting with petroleum ether / ethyl acetate = 1:20) and the residue was purified by column chromatography to give a white solid 3 aa;
[0028] White solid (75%, 72.5 mg) mp:. 19...
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[0029] Example 2:
[0030] 9- (o-toluenesulfonyl) -9 H - xanthene (3Ba) Synthesis and Characterization:
[0031]
[0032] Respectively, 0.6 mmol 2- methyl-benzene sulfonyl hydrazide, 0.3 mmol 9 H - xanthene, 0.06 mmol of potassium iodide and cesium carbonate 0.6mmol was added 25 mL three-neck flask, was added 6 mL 1,2- dichloroethane and hexafluoroisopropanol mixture (v: v = 4: 2) dissolved carbon rod as the anode, the platinum plate as the cathode, the reaction mixture was stirred for 4 hours at a constant current of 12 mA at normal temperature, TLC monitoring of the reaction progress;
[0033] After completion of the reaction, the mixture was extracted with ethyl acetate (10 mL). The organic layer was dried over anhydrous Na 2 SO 4 Drying, rotary evaporation under reduced pressure, and (silica gel eluting with petroleum ether / ethyl acetate = 1:30) and the residue was purified by column chromatography to give a white solid 3Ba;
[0034] White solid (44%, 44.4 mg) mp:. 216.7-2...
Example Embodiment
[0035] Example 3:
[0036] 9- (m-toluenesulfonyl) -9 H - xanthene (3Ca) Synthesis and Characterization:
[0037]
[0038] Respectively, 0.6 mmol 3- methylbenzene sulfonyl hydrazide, 0.3 mmol 9 H - xanthene, 0.06 mmol tetrabutylammonium iodide and 0.6 mmol of sodium methoxide was added to 25 mL three-neck flask, was added 6 mL 1,2- dichloroethane and hexafluoroisopropanol mixture (v: v = 4: 2) was dissolved, with the carbon rod as the anode, the platinum plate as the cathode, is carried out at a constant current of 15 mA, with stirring at room temperature to react for 5 h, TLC monitoring of the reaction progress;
[0039] After completion of the reaction, the mixture was extracted with ethyl acetate (10 mL). The organic layer was dried over anhydrous Na 2 SO 4Drying, rotary evaporation under reduced pressure, and (silica gel eluting with petroleum ether / ethyl acetate = 1:40) and the residue was purified by column chromatography to give a white solid 3Ca;
[0040] White solid (7...
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