反应详情

温度

100 °C

A mixture of (3R,5S)-3,5-dimethylpiperazine-1-sulfonamide (the product of example 72, 0.26 g), tris(dibenzylideneacetone)-dipalladium (0) (61 mg), 2-dicyclohexylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (XPHOS) (32 mg), cesium carbonate (0.32 g) and 4-chloro-2-[[(2,3-difluorophenyl)methyl]thio]-6-methoxypyrimidine (the product of example 35 step i, 0.20 g) in anhydrous dioxane (8 ml) was heated at reflux in a microwave at 100° C., 300 W, open vessel with cooling for 15 min. Saturated aqueous ammonium chloride (5 ml) and EtOAc (5 ml) were added, followed by H2O. The layers were separated and the organic layer extracted with H2O (×3). The organic layer was discarded and the combined aqueous extracts exhaustively extracted with further EtOAc. These extracts were combined, washed with saturated aqueous sodium chloride, dried with sodium sulfate, filtered and evaporated. The resulting solid was washed with H2O to afford the title compound as a white solid. Yield: 0.111 g

1. temperaturewas heated
2. temperature300 W, open vessel with cooling for 15 min
3. customThe layers were separated
4. extractionthe organic layer extracted with H2O (×3)
5. extractionthe combined aqueous extracts exhaustively extracted with further EtOAc
6. washwashed with saturated aqueous sodium chloride
7. dry with materialdried with sodium sulfate
8. filtrationfiltered
9. customevaporated
10. washThe resulting solid was washed with H2O