4-BROMO-7-BROMOQUINOLINE synthesis

Yield:700871-88-1 75%

Reaction Conditions:

with lithium bromide in acetonitrile at 55; for 8 h;under nitrogen;

Steps:

22 4,7-Dibromoquinoline

The product of Preparation 20 (3.15 g, 8.8 mmol) and LiBr (7.7 g, 88.5 mmol) are dissolved in 100 mL OF CH3CN and the mixture is heated at 55 °C for 8 h under nitrogen. The reaction mixture is cooled to RT and evaporated to a slurry. The crude mixture is diluted with EtOAc (30 mL) and washed with saturated NAHC03 solution. The organic phase is separated and extracted with saturated brine, dried (NA2S04), filtered, and evaporated to a solid mass. The crude product is purified by MPLC on silica gel (25% ETOAC/HEXANES) to yield the title compound, 1.9 g (75%), as white solid. MS ES+ m/e 287.8 (M+1).

References:

WO2004/48383,2004,A1 Location in patent:Page 51