ChemicalBook CAS DataBase List 4,4'-DIBROMO-2,2'-BIPYRIDINE

4,4'-DIBROMO-2,2'-BIPYRIDINE synthesis

7synthesis methods

Product Name:4,4'-DIBROMO-2,2'-BIPYRIDINE
CAS Number:18511-71-2
Molecular formula:C10H6Br2N2
Molecular Weight:313.98

4,4'-DIBROMO-2,2'-BIPYRIDINE-N,N'-DIOXIDE

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18511-71-2
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Yield:18511-71-2 77%

Reaction Conditions:

with phosphorus tribromide in chloroform at -3 - 60; for 2 h;Inert atmosphere;

Steps:

4.4

A 2 L round-bottom flask was substituted with nitrogen gas, and 37 g of Formula 4-c (0.1 mol) was added thereto, and dissolved by addition of 950 mL of chloroform. At -3° C., 297 g of tribromophosphine (1.1 mol) was slowly dropwise added thereto, followed by stirring at 60° C., for 2 hours. The resultant product was cooled to room temperature, added to 1 L of water, added with caustic soda until pH reached 11, and extracted with methylene chloride. Then, an organic layer was separated. After removal of moisture, and removal of a solvent by vacuum distillation, the precipitated solid was washed with ethanol, and filtered so as to provide a pale yellow solid, 26 g of Formula 4-d (yield 77%).

References:

US2012/247546,2012,A1 Location in patent:Page/Page column 35