反应详情

温度

120 °C

A mixture of 2-(2-chloropyrimidin-5-yl)-1,1,1,3,3,3-hexafluoropropan-2-ol (490 mg, 1.747 mmol, Intermediate D), 1-((6-chloropyridin-3-yl)sulfonyl)-3-(prop-1-yn-1-yl)piperazine (325 mg, 1.08 mmol), Hünig's base (1.0 mL, 5.73 mmol) and dioxane (5.0 mL) was heated at 120° C. for 15 h. The temperature was increased to 130° C. and stirring was continued for 24 h. The dark mixture was allowed to cool to room temperature and was then purified by silica gel chromatography (80 g silica gel, 10-50% EtOAc in hexane) to give 2-(2-(4-((6-chloro-3-pyridinyl)sulfonyl)-2-(1-propyn-1-yl)-1-piperazinyl)-5-pyrimidinyl)-1,1,1,3,3,3-hexafluoro-2-propanol as a white foam (0.664 g).

1. temperatureThe temperature was increased to 130° C.
2. temperatureto cool to room temperature
3. customwas then purified by silica gel chromatography (80 g silica gel, 10-50% EtOAc in hexane)