反应详情

A solution of intermediate 82 (200 mg, 0.7 mmol), 1H-pyrazole (95 mg, 2 eq), CuI (133 mg, 1 eq), K2CO3 (290 mg, 2.1 eq) and (1R,2R)-diaminomethylcyclohexane (100 mg, 1 eq) in anh. NMP (1 mL), under N2, was heated at 150° C. for 6 hr. It was cooled down to r.t. and poured into water. EtOAc was added and the phases were separated. The aqueous layer was further extracted with EtOAc (2×10 mL). The combined organic extracts were dried over anh. Na2SO4, the solids were filtered and the solvent evaporated. The residue was purified by flash-chromatography (silica gel, cHex/EtOAc 8:2) to give the title compound as a white solid (85.6 mg, 70%).

1. customthe phases were separated
2. extractionThe aqueous layer was further extracted with EtOAc (2×10 mL)
3. dry with materialThe combined organic extracts were dried over anh. Na2SO4
4. filtrationthe solids were filtered
5. customthe solvent evaporated
6. customThe residue was purified by flash-chromatography (silica gel, cHex/EtOAc 8:2)