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ChemicalBook CAS DataBase List 2-BROMOTHIOPHENE-3-CARBALDEHYDE

2-BROMOTHIOPHENE-3-CARBALDEHYDE synthesis

6synthesis methods
-

Yield:1860-99-7 78.8%

Reaction Conditions:

with 1-hydroxy-3H-benz[d][1,2]iodoxole-1,3-dione in dimethyl sulfoxide at 60 - 70;Inert atmosphere;

Steps:

1.3 3, Preparation of compound 2-bromo-3-thiophenecarboxaldehyde
In a 250 ml two-necked flask, 11.9 g of 2-bromo-3- (bromomethyl) thiophene (256 g mol- 1, 11.9 g, 46 mmol)Pump without water treatment.Under N2 protection, 20.8 g of IBX (280 g mol-1, 20.8 g, 74 mmol, 1.6 equiv)Add 130ml anhydrous DMSO, 60-70°C oil bath for 3-4 hours.After treatment: add 20ml of deionized water to quench the reaction. The mixture was extracted with dichloromethane, washed with a large amount of methylene chloride, and precipitated as a white solid. The filtrate was collected by suction filtration, dried and concentrated by column chromatography.Eluent petroleum ether / ethyl acetate 40: 1 (V: V).

References:

Wuhan University of Technology;Xiao Shengqiang;Chen Run;You Wei;Zhan Chun CN106588868, 2017, A Location in patent:Paragraph 0025; 0034; 0035; 0036; 0037

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