反应详情

To an ice-bath cooled solution of Intermediate 103e (97 mg, 0.13 mmol) in DCM (2 mL) was added DIPEA (58 μL, 0.32 mmol) followed by methanesulfonyl chloride (22 μL, 0.27 mmol). The reaction mixture was stirred for 2 h 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 to afford the title compound (130 mg, quantitative). LCMS (Method 1): Rt 3.69 min, m/z 759 [MH+].

1. customthen 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