8-chloro-3-iodo-2-MethyliMidazo[1,2-a]pyrazine synthesis

Yield:1334167-35-9 97%

Reaction Conditions:

with N-iodo-succinimide;acetic acid in dichloromethane at 0 - 20; for 16 h;

Steps:

A25

N-Iodosuccinimide (14.1 g, 62 mmol) was added to a stirred solution of intermediate 4 (9.58 g, 57 mmol) in a mixture of DCM and acetic acid at 0 °C. The mixture was allowed to warm to RT and then stirred for 16 h. The mixture was diluted with further DCM and washed with a saturated solution of sodium carbonate and sodium thiosulfite. The organic layer was separated, dried (Na₂S0₄), filtered and the solvents evaporated in vacuo. The crude product was precipitated from diisopropyl ether to yieldintermediate 25 (16 g, 97%) as a pale brown solid which was used in the next step without further purification.

References:

WO2011/110545,2011,A1 Location in patent:Page/Page column 80