反应详情

To a solution of 3-t-butyloxycarbonylamino-3,4-dihydro-1H-1-benzazepine-2,5-dione (500 mg, 1.72 mmol) in 25 ml anhydrous DMF was-added cesium carbonate (562 mg) followed by iodomethane (215 μl). The reaction was stirred for one hour, diluted with ethyl acetate and then washed with water. The organic phase was separated, washed with brine, dried (MgSO4) and concentrated to give a yellow solid. Tritiation with diethyl ether gave 3-t-butyloxycarbonylamino-1-methyl-3,4-dihydro-1H-1-benzazepine-2,5-dione as a colourless solid. 1H NMR (250 MHz, CDH3) δ 7.64-7.50 (M, 2H) 7.38-7.24 (t, 1H) 7.20-7.60 (d, 1H,) 5.78-5.66 (br d, 1H,) 4.98-4.82 (M, 1H) 3.40 (s, 3H) 3.36-3.20 (dd, 2H) 2.98-2.80 (dd, 2H).

1. washwashed with water
2. customThe organic phase was separated
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customto give a yellow solid