反应详情

To a suspension of 2-(2-isopropyl-2H-[1,2,4]triazol-3-yl)-8-piperidin-4-yl-4,5-dihydro-6-oxa-1,3a-diaza-benzo[e]azulene trifluoroacetic acid salt (300 mg, 0.61 mmol) in THF (5 mL) was added potassium carbonate (295 mg, 2.13 mmol) and N-tert-butyl-2-chloro-acetamide (100 mg, 0.67 mmol). The mixture was stirred for 5 days before being diluted with DCM and washed with water (2×30 mL). The organic phase was dried (MgSO4) and concentrated in vacuo. The resultant residue was triturated in diethyl ether, affording 274 as a cream solid (169 mg, 0.34 mmol, 56%). LCMS: RT=3.12 min, [M+H]+=492. 1H NMR δ (ppm) (DMSO-d): 8.29 (1 H, d, J=8.29 Hz), 7.86 (1 H, d, J=0.63 Hz), 7.85 (1 H, s), 7.15 (1 H, s), 7.03 (1 H, dd, J=8.36, 1.77 Hz), 6.89 (1 H, d, J=1.71 Hz), 5.90-5.80 (1 H, m), 4.48-4.41 (4 H, m), 2.85 (2 H, d, J=11.24 Hz), 2.81 (2 H, s), 2.20-2.09 (2 H, m), 1.78-1.67 (2 H, m), 1.70-1.58 (2 H, m), 1.44 (6 H, d, J=6.60 Hz), 1.25 (9 H, s). 1H obscured by solvent.

1. washwashed with water (2×30 mL)
2. dry with materialThe organic phase was dried (MgSO4)
3. concentrationconcentrated in vacuo
4. customThe resultant residue was triturated in diethyl ether