反应详情

To a suspension of 0.63 g (3.26 mmol) 2-(3H-imidazo[4,5-b]pyridin-3-ylmethoxy)-ethanol and 1.71 g (6.52 mmol) triphenylphosphine in 10 ml pyridine kept under argon were added dropwise over 10 min. 0.32 ml (3.32 mmol) CCl4. The suspension was stirred at room temperature for 18 hours and concentrated in vacuo. The crude product was purified by flash chromatography (silica gel, gradient DCM→DCM/MeOH 9/1) and triturated with diethylether to afford 0.7 g of a brownish solid. MS(ISP): 212.1 [MH]+.

1. additionwere added dropwise over 10 min
2. concentrationconcentrated in vacuo
3. customThe crude product was purified by flash chromatography (silica gel, gradient DCM→DCM/MeOH 9/1)
4. customtriturated with diethylether