1-BroMo-2-(isopropanesulfonyl)benzene synthesis

Yield:900174-43-8 96%

Reaction Conditions:

Stage #1: o-bromothiophenol;isopropyl bromidewith potassium carbonate in dichloromethane at 38 - 40; for 5 h;
Stage #2: with dihydrogen peroxide in dichloromethane at 25 - 30; for 6 h;

Steps:

13 Example 13: Preparation of 2-isopropylsulfonylbromobenzene (IX1)

To a 500 ml four-necked flask equipped with a stirring and thermometer, 300 g of dichloromethane, 36.0 g of potassium carbonate, 37.5 g (0.2 mol) of 2-bromothiophenol, and 36.5 g (0.3 mol) of 2-bromopropane were added. The reaction was stirred at 38-40 ° C for 5 hours, cooled to 20-25 ° C, filtered, and the filter cake was washed twice with dichloromethane, 40 g each time, the filtrate was combined, and the filtrate was transferred to another 1000 ml four-neck flask and added. 70.0 g (0.62 mol) of 30% hydrogen peroxide, stirred at 25-30 ° C for 6 hours, layered, the aqueous layer was extracted twice with dichloromethane, 20 g each time, the organic phase was combined, washed once with 50 g of 5% aqueous sodium sulfite solution 50 g of saturated aqueous sodium chloride solution was washed once, dichloromethane was distilled off, 100 g of methyl tert-butyl ether, 0.5 g of activated carbon was added to the residue, decolorized, filtered, and recrystallized to obtain 50.5 g of 2-isopropylsulfonyl group. Bromobenzene, the yield was 96.0%, and the liquid phase purity was 99.1%.

References:

CN109748885,2019,A Location in patent:Paragraph 0110; 0111