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ChemicalBook CAS DataBase List NSC44969
73006-78-7

NSC44969 synthesis

13synthesis methods
-

Yield:73006-78-7 90%

Reaction Conditions:

with bis-triphenylphosphine-palladium(II) chloride;potassium carbonate in 1,2-dimethoxyethane;water; for 16 h;Reflux;

Steps:

1

4-chloro-2-iodoaniline (90 g, 355 mmol), phenylboronic acid (52.0 g, 426 mmol), potassium carbonate (147 g, 1065 mmol), DME (720 ml) and water (720 ml) were added to a 5 L flask. After degassing, bis(triphenylphosphine)palladium(II) chloride (4.98 g, 7.10 mmol) was added to the mixture and refluxed for 14 hours. After completion, the reaction mixture was diluted with EtOAc (1 L).And separate the two layers. The aqueous layer was extracted with EtOAc (EtOAc m.The resulting oil was purified by column chromatography using EtOAc /hexanes.5-Chloro-[1,1'-biphenyl]-2-amine (90% yield) was obtained.

References:

CN110128479,2019,A Location in patent:Paragraph 0323; 0324