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ChemicalBook CAS DataBase List 2'-BROMO-4-CHLORO-BIPHENYL

2'-BROMO-4-CHLORO-BIPHENYL synthesis

10synthesis methods
-

Yield:179526-95-5 94%

Reaction Conditions:

with tetrakis-(triphenylphosphine)-palladium;potassium carbonate in ethanol;lithium hydroxide monohydrate;toluene at 80; for 4 h;Inert atmosphere;

Steps:

1.4 Intermediate E was synthesized by Reaction Scheme 4-1 below:

In an argon atmosphere, in a 1 L three-neck flask, 1-bromo-2-iodobenzene (25.0 g), 4-chlorophenylboronic acid (13.8 g), Pd(PPh3)4 (5.1 g), and K2CO3 (24.4 g) were added and dissolved in a mixed solvent of toluene, water, and ethanol (10:2:1, 350 mL), and the mixture was heated and stirred at about 80° C. for about 4 hours. The resultant mixture was extracted with CH2Cl2 by adding water to obtain organic layers. The obtained organic layers were combined and dried over MgSO4, and the solvent was removed by distillation under reduced pressure. The resulting crude product was purified by silica gel column chromatography to obtain Intermediate E (22.1 g, yield: 94%). The molecular weight of Intermediate E measured by FAB-MS measurement was 267.

References:

US2022/131079,2022,A1 Location in patent:Paragraph 0204; 0218-0220