反应详情

To a mixture of cyclopropanesulfonic acid [14-amino-18-(isoquinolin-1-yloxy)-2,15-dioxo-3,16-diaza-tricyclo[14.3.0.04,6]nonadec-7-ene-4-carbonyl]-amide bis hydrochloride (50 mg, 0.075 mmol) in 2 mL of DCM was added 44 μL (0.25 mmol)of DIPEA and 9 mg (0.10 mmol) of methyl chloroformate. The mixture was stirred at rt for 2 h. It was then diluted with EtOAc and washed with pH 4 buffer (2×) and brine (1×). The organic phase was dried (MgSO4) and concentrated in vacuo to give the crude product. Flash chromatography (2% MeOH/DCM) gave 40 mg (82%) of the desired product as a white solid: LC-MS (Method A, retention time: 3.05 min), MS m/z 654 (M++1).

1. washwashed with pH 4 buffer (2×) and brine (1×)
2. dry with materialThe organic phase was dried (MgSO4)
3. concentrationconcentrated in vacuo
4. customto give the crude product