反应详情

To a solution of the ester 124 (473 mg, 1.02 mmol) in DMF (15 ml) was added 60% NaH (45 mg, 1.12 mmol). The solution was stirred for one hour at room temperature under nitrogen, cooled to 0° C., treated with MeI (170 μl, 1.12 mmol), warmed to room temperature and stirred overnight under nitrogen. The mixture was partitioned between water and AcOEt, organic layer was collected, dried over MgSO4 and concentrated in vacuo to yield 454 mg (93%). 1H-NMR (DMSO) δ: 7.99 (m, 1H), 7.56 (dd, J=1.4, 8.2 Hz, 1H); 7.47 (m, 1H); 7.27 (s, 1H); 6.86 (d, J=8.8 Hz, 2H); 6.75 (d, J=9.0 Hz, 2H); 4.86 (s, 2H); 3.83 (s, 3H); 3.76 (s, 3H); 3.67 (t, J=4.8 Hz, 4H); 3.01 (t, J=4.8 Hz, 4H); 1.37 (s, 9H).

1. temperaturecooled to 0° C.
2. temperaturewarmed to room temperature
3. stirringstirred overnight under nitrogen
4. customThe mixture was partitioned between water and AcOEt, organic layer
5. customwas collected
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customto yield 454 mg (93%)