反应详情

A solution of 2-(2,4-difluorophenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine (3.25 g, 13.9 mmol, prepared using General Procedure R from Example #8, Step A with 2-iminopiperidine hydrochloride), NIS (3.12 g, 13.9 mmol), and DMF (35 mL) was stirred at ambient temperature. After stirring overnight, the reaction mixture was partitioned between Et2O (400 mL) and water (200 mL). The organic phase was separated and dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified by silica gel chromatography using heptane/EtOAc (gradient from 100:0 to 0:100) to give the title compound (3.44 g, 69%). LC/MS (Table 1, Method a) Rt=3.32 min; MS m/z: 361.0 (M+H)+.

1. customthe reaction mixture was partitioned between Et2O (400 mL) and water (200 mL)
2. customThe organic phase was separated
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by silica gel chromatography