反应详情

温度

100 °C

A mixture of tert-Butyl 4-(aminosulfonyl)-1,4-diazepane-1-carboxylate (the product of example 75, 0.277 g), tris(dibenzylideneacetone)-dipalladium (0) (45 mg), 2-dicyclohexylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (XPHOS) (24 mg), cesium carbonate (0.242 g) and 4-chloro-2-[[(2,3-difluorophenyl)methyl]thio]-6-methoxypyrimidine (the product of example 35 step i, 0.15 g) in anhydrous dioxane (6 ml) was heated at reflux in a microwave at 100° C., 300 W, open vessel with cooling for 15 min. Saturated aqueous ammonium chloride was added and the resulting mixture extracted with EtOAc. The combined organic extracts were washed with saturated aqueous sodium chloride, dried with sodium sulfate, filtered and evaporated. The residue was purified by column chromatography on silica using a 1:19 to 3:7 mixture of EtOAc and iso-hexane as eluent to give the subtitle compound as a yellow oil. Yield: 0.223 g

1. temperaturewas heated
2. temperature300 W, open vessel with cooling for 15 min
3. extractionthe resulting mixture extracted with EtOAc
4. washThe combined organic extracts were washed with saturated aqueous sodium chloride
5. dry with materialdried with sodium sulfate
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by column chromatography on silica using a 1:19
9. additionto 3:7 mixture of EtOAc and iso-hexane as eluent