反应详情

To a solution of Intermediate 122a (240 mg, 1.38 mmol) and (5-fluoro-pyridin-2-yl)-hydrazine (176 mg, 1.38 mmol) in DCM (10 mL) was added DIPEA (721 μL, 4.15 mmol) and the reaction stirred for 5 days. The reaction was then partitioned between DCM and water. The aqueous phase was extracted with DCM (×3) and the combined organic layers were washed with brine, dried (MgSO4) and concentrated in vacuo. The resultant residue was purified by FCC on silica, using a gradient of 0-10% MeOH in DCM to give the title compound (170 mg, 47%). LCMS (Method 3): Rt 2.31 min, m/z 265 [MH+].

1. customThe reaction was then partitioned between DCM and water
2. extractionThe aqueous phase was extracted with DCM (×3)
3. washthe combined organic layers were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe resultant residue was purified by FCC on silica