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ChemicalBook CAS DataBase List 2,5-DIBROMO-3-CHLOROPYRIDINE

2,5-DIBROMO-3-CHLOROPYRIDINE synthesis

2synthesis methods
97966-00-2 Synthesis
5-Bromo-2,3-dichloropyridine

97966-00-2
195 suppliers
$10.00/1g

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Yield: 80%

Reaction Conditions:

with hydrogen bromide in acetic acid at 70; for 7 h;

Steps:

12.1 2,5-dibromo-3-chloropyridine
To 5-bromo-2,3-dichloropyridine (29) (11.7 g, 51.6 mmol) was added HBr (5M in AcOH) (51.6 ml, 258 mmol) at room temperature. Then the reaction mixture was heated to 70° C. After being stirred for 7 hrs at 70° C., the reaction mixture was diluted with ethyl acetate, quenched with H2O and extracted with ethyl acetate. The resulting organic layer was washed with 1M NaOH, dried over over Na2SO4 and concentrated in vacuo. The residue was recrystallized from hexane-ethyl acetate to afford 11.2 g of the desired product (41) in 80% yield as a white solid. 1H-NMR (DMSO-d6) δ: 8.55 (1H, s), 8.49 (1H, s).

References:

SHIONOGI & CO., LTD.;Kurose, Noriyuki;Iso, Yasuyoshi;Yamaguchi, Naoko;Shao, Bin;Tafesse, Laykea;Zhou, Xiaoming;Yu, Jianming US9156830, 2015, B2 Location in patent:Page/Page column 104

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