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ChemicalBook CAS DataBase List 4-BroMo-2-chloro-1-Methanesulfonylbenzene

4-BroMo-2-chloro-1-Methanesulfonylbenzene synthesis

4synthesis methods
-

Yield:648905-09-3 52.6%

Reaction Conditions:

in methanol;water at 40;

Steps:

5.B Step B. 4-bromo-2-chloro-l-(methylsulfonyl)benzene

Step B. 4-bromo-2-chloro-l-(methylsulfonyl)benzene A mixture of (4-bromo-2-chlorophenyl)(methyl)sulfane (5 g, 21.3 mmol) and oxone (39 g, 63.8 mmol) in MeOH/H20 (50 mL/50 mL) was stirred at 40 °C overnight. The reaction mixture was concentrated under reduced pressure to remove MeOH. The resulting aqueous mixture was extracted with EtOAc (40 mL x 3). The extracts were combined, washed with brine (50 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography using petroleum ether :EtO Ac (3 : 1) as eluting solvents to afford 4-bromo-2-chloro-l- (methylsulfonyl)benzene as a white solid (3 g, 52.6%), which was used for the next step without further purification. LCMS (ESI) m/z: 270.0 [M+H]+.

References:

WO2015/100617,2015,A1 Location in patent:Page/Page column 39