反应详情

A mixture of 4-chloro-7-(3-(trifluoromethyl)pyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (0.100 g, 0.000314 mol) tris(dibenzylideneacetone)dipalladium(0) (0.058 g, 0.000063 mol), Cesium Carbonate (0.311 g, 0.000944 mol) and Xantphos (0.018 g, 0.000031 mol) in 1,4-Dioxane (3 mL, 0.04 mol) was stirred at room temperature for 10 minutes in a 5 mL microwave vial. 4-(trifluoromethylsulfonyl)benzenamine (0.15 g, 0.00063 mol) was then added as a solution in dioxane (0.5 mL) and the mixture was stirred for an additional 5 minutes. The mixture was heated via microwave in a sealed tube at 140° C. for 30 minutes, allowed to cool, and reduced in vacuo. The resulting black solid was taken up in ethyl acetate (50 mL) and washed with brine and water (2×50 mL), dried over magnesium sulfate, and reduced in vacuo. The mixture was purified by flash chromatography using an ethyl acetate:hexanes (0-100%) gradient. The combined pure fractions were reduced in vacuo to yield the desired product as a tan solid (0.087 g).

1. stirringthe mixture was stirred for an additional 5 minutes
2. temperatureThe mixture was heated via microwave in a sealed tube at 140° C. for 30 minutes
3. temperatureto cool
4. washwashed with brine and water (2×50 mL)
5. dry with materialdried over magnesium sulfate
6. customThe mixture was purified by flash chromatography