反应详情

The product of Step 2 (64 mg, 0.14 mmol) is suspended in dichloromethane (0.5 mL), trifluoroacetic acid (0.25 mL) and H2O (3 drops). The reaction mixture is stirred and room temperature for 40 min. The mixture is purged with nitrogen and then basified to pH 9 with 2M NaOH (aq.). The aqueous layer is extracted with dichoromethane and ethyl acetate. The combined organics are dried (MgSO4) and solvent is removed in vacuo to yield the title compound as an off-white solid (10 mg, 20%). 1H-NMR (400 MHz, d6-DMSO) =1.13 (t, 2H, J=6.8), 1.57-1.70 (m, 2H), 2.58-2.72 (m, 2H), 3.02-3.08 (m, 2H), 4.13-4.30 (m, 1H), 4.50 (s, 2H), 7.81 (d, 1H, J=8), 7.92 (s, 1H), 8.03-8.11 (m, 2H), 8.18 (s, 1H), 8.63 (s, 1H), 8.69 (s, 1H). LCMS: Rt 6.55 min (86.9%), m/z (APCI) 350 (M+H)+.

1. customThe mixture is purged with nitrogen
2. extractionThe aqueous layer is extracted with dichoromethane and ethyl acetate
3. dry with materialThe combined organics are dried (MgSO4) and solvent
4. customis removed in vacuo