反应详情

The product of step 2 (50 mg, 0.11 mmol) and sodium methanesulfinate (23 mg, 0.22 mmol) in dimethylformamide (1 mL) is heated at 60° C. for 1 hour. The solvent is removed under reduced pressure and DCM (1 mL) is added, followed by trifluoroacetic acid (0.25 mL). The reaction mixture is stirred at room temperature for 3 hours. The reaction mixture is diluted with toluene (5 mL) then the solvent removed under reduced pressure. The crude material is purified using HPLC (5 to 95 acetonitrile/water) to give title compound (17 mg): 1H NMR (400 MHz, DMSO-d6) δ:3.03 (s, 3H), 4.15-4.34 (m, 1.5H), 4.38-4.46 (m, 0.5H), 4.55-4.62 (m, 0.5H), 4.65-4.76(m, 2.5H), 4.89 (t, J=4.0 Hz, 1H), 6.00 (d, J=4.0 Hz, 1H), 6.53 (s, 1H), 7.49(d, J=8.0 Hz, 2H), 7.58 (d, J=8.0 Hz, 1H), 7.72 (d, J=8.0 Hz, 2H), 8.11-8.17 (m, 1H), 8.62 (d, J=8.0 Hz, 1H), 8.90 (bs, 1H). m/z (Cl) 449 [M+H].

1. customThe solvent is removed under reduced pressure and DCM (1 mL)
2. additionis added
3. additionThe reaction mixture is diluted with toluene (5 mL)
4. customthe solvent removed under reduced pressure
5. customThe crude material is purified