反应详情

温度

140 °C

To a solution of 4-chloro-1H-pyrrolo[2,3-d]pyrimidine (1.69 g, 11.0 mmol) and TEA (4.60 mL, 33.0 mmol) in 1-butanol (25.0 mL) was added benzenethiol (3.39 mL, 33.0 mmol), and the mixture was refluxed at 140° C. overnight. The reaction was then cooled to rt and concentrated in vacuo. The off-white solid was purified by silica gel chromatography eluting with a gradient of 0 to 35% EtOAc in DCM to afford the product (2.29 g, 92%). LC/MS: Rt=1.55 min, ES+ 228 (FA standard).

1. temperatureThe reaction was then cooled to rt
2. concentrationconcentrated in vacuo
3. customThe off-white solid was purified by silica gel chromatography
4. washeluting with a gradient of 0 to 35% EtOAc in DCM