反应详情

温度

65 °C

Under a N2 atmosphere, 150 mg (0.334 mmol) of 1-(3-bromo-4-ethyl-anilino)-4-[2-(2-hydroxy-pyridin-4-yl)-ethyl]-isoquinoline (Ex. 32a) in 5 ml of acetonitrile are mixed with 76 μl (0.83 mmol) of phosphorus oxychloride and 0.17 ml (0.68 mmol) of 4 N HCl in dioxane, and stirred at 65° C. A further 76 μl of phosphorus oxychloride is added after 12 h, and stirring continues for 48 h at 65° C. The mixture is cooled to RT, 4 ml of 10% NH3 solution added, and it is partitioned between 3 portions of EtOAc, 2 portions of water and brine. Drying (Na2SO4), concentrating by evaporation and chromatography on silica gel (acetone/methylene chloride 3:2) yield 1-(3-bromo-4-ethyl-anilino)-4-[2-(2-chloro-pyridin-4-yl)ethyl]-isoquinoline; FAB-MS: (M+H)+=466/468; HPLC(gradient20-100) tRef=13.4.

1. stirringstirring
2. temperatureThe mixture is cooled to RT
3. customit is partitioned between 3 portions of EtOAc, 2 portions of water and brine
4. dry with materialDrying (Na2SO4)
5. concentrationconcentrating by evaporation and chromatography on silica gel (acetone/methylene chloride 3:2)