反应详情

To an ice-bath cooled solution of Intermediate 106a (150 mg, 0.25 mmol) in DCM (3 mL) was added DIPEA (107 μL, 0.61 mmol) followed by methanesulfonyl chloride (29 μL, 0.37 mmol). The reaction mixture was stirred for 2 h. After warming to RT, additional amount of DIPEA (65 μL) and methanesulfonyl chloride (30 μL) were added and stirring was continued for 2 h. The reaction mixture was 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 (Quantitative). Product used in the following step without further purification. LCMS (Method 4): Rt 3.59 min, ink 653 [MH+].

1. stirringstirring
2. waitwas continued for 2 h
3. customThe reaction mixture was partitioned between DCM and water
4. extractionThe aqueous phase was extracted with DCM (×3)
5. washthe combined organic layers were washed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo