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ChemicalBook CAS DataBase List 4,4''-Dichloro-1,1':2',1''-terphenyl
21711-56-8

4,4''-Dichloro-1,1':2',1''-terphenyl synthesis

7synthesis methods
4-Chlorophenylboronic acid

1679-18-1

1,2-Dibromobenzene

583-53-9

4,4''-Dichloro-1,1':2',1''-terphenyl

21711-56-8

Under nitrogen protection, 1,2-dibromobenzene (20.0 g, 84.78 mmol), 4-chlorophenylboronic acid (30.49 g, 194.99 mmol), tetrakis(triphenylphosphine)palladium (4.89 g, 4.24 mmol) and potassium carbonate (28.10 g, 203.33 mmol) were dissolved in a mixed solvent of toluene (150 mL), water (150 mL) and ethanol ( 150 mL) in a solvent mixture. The reaction mixture was stirred at 100 °C for 5 hours. After completion of the reaction, the reaction mixture was extracted with dichloromethane, the organic phases were combined and concentrated under reduced pressure. Purification by column chromatography afforded 19.5 g of the target product 4,4''-dichloro-1,1':2',1''-terphenyl.

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Yield:21711-56-8 19.5 g

Reaction Conditions:

with tetrakis(triphenylphosphine) palladium(0);potassium carbonate in ethanol;water;toluene at 100; for 5 h;Inert atmosphere;

Steps:

1 Preparation 1: Synthesis of a-1

Under a nitrogen stream1,2-dibromobenzene (20.0 g, 84.78 mmol),4-chlorophenyl boronic acid (30.49 g, 194.99 mmol), Pd (PPh3) 4 (4.89 g, 4.24 mmol) and K2CO3 (28.10 g, 203.33 mmol) were mixed with 150 ml of toluene, 150 ml of H2O and 150 ml of ethanol And the mixture was stirred at 100 degree For 5 hours. After completion of the reaction, the mixture was extracted with methylene chloride, concentrated under reduced pressure, and 19.5 g of a-1 was obtained by column chromatography.

References:

KR2015/103949,2015,A Location in patent:Paragraph 0055-0057