反应详情

温度

100 °C

A mixture of azetidine-1-sulfonamide (0.27 g), tris(dibenzylideneacetone)dipalladium (0) (50 mg), 2-dicyclohexylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (XPHOS) (50 mg), cesium carbonate (0.43 g) and (trans)-2-{6-chloro-2-[(2,3-difluorobenzyl)thio]pyrimidin-4-yl}cyclopentanol (the product from step i), 0.50 g) in dioxane (20 ml) was heated at reflux in a microwave at 100° C., 300 W, open vessel with cooling for 1 h. The reaction mixture was then reduced in vacuo and the residue partitioned between DCM (150 ml) and H2O (150 ml). The organics were separated and the aqueous layer was re-extracted with DCM (2×150 ml). Organics were combined, dried (MgSO4) and reduced under vacuo and the resulting residue purified by prep HPLC to give the title compound as a white solid. Yield 74 mg

1. temperaturewas heated
2. temperature300 W, open vessel with cooling for 1 h
3. customthe residue partitioned between DCM (150 ml) and H2O (150 ml)
4. customThe organics were separated
5. extractionthe aqueous layer was re-extracted with DCM (2×150 ml)
6. dry with materialdried (MgSO4)
7. customthe resulting residue purified by prep HPLC