3,5-dibroMo-2-broMoMethyl-pyridine synthesis

Yield:1227502-56-8 55%

Reaction Conditions:

with N-Bromosuccinimide;2,2'-azobis(isobutyronitrile) in tetrachloromethane; for 4 h;Heating / reflux;

Steps:

52B

To a solution of 52A (1.25 g, 4.98 mmol) in CCl₄ (7 ML) was added NBS (0.89 g, 4.98 mmol) followed by catalytic AIBN and the mixture was heated to reflux for 4 hours. The reaction was cooled to room temperature, filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO₂, 10% CH₂Cl₂/Hexane then 50% CH₂Cl₂/Hexane) to give 52B (0.90 g, 55%). HPLC R_t=2.85 min.

References:

US2005/192310,2005,A1 Location in patent:Page/Page column 35