Preparation method of tetrahydro-cyclopentyl[2,1-b;3,4-b'] bi-thiophene ketone
A technology of 4-b and thiophenone, applied in the field of 4hydro-cyclopenta[2, can solve the problems of long reaction steps, harsh reaction conditions, and low yield, and achieve the effect of easy realization and mild conditions
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[0023] (1) Preparation of 3-methyl 2,2'-bithiophene
[0024] Add 3.54g (20mmol) 2-bromo-3-methylthiophene, 3.84g (30mmol) 2-thiophene boronic acid, 52.4mg (0.2mmol) triphenylphosphine, 100ml tetrahydrofuran, 100ml (2mol / L) into a 250ml three-necked flask Potassium carbonate solution was protected by argon, and after stirring, 65mg of palladium acetate was added, heated to 65°C and refluxed for 4h. Stop heating, lower to room temperature, extract the reaction system 3 times with 200ml toluene, combine the organic phases, wash the organic phases with saturated aqueous sodium chloride until neutral, then dry the organic phases with anhydrous magnesium sulfate, and filter the organic phases , the filtrate was concentrated, and then the concentrate was subjected to column chromatography to obtain 3.3 g of a colorless liquid, yield: 92%.
[0025] Structure Identification:
[0026] 1 H NMR (500MHz, CD 3 COCD 3 ): 2.36(m, 3H), 6.94(d, 1H), 7.11(t, 1H), 7.18(dd, 1H), 7.30(d, 2H), ...
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