反应详情

2-(4-methyl-5-oxo-2,5-dihydrofuran-3-yl)-2,8-diazaspiro[4.5]decan-1-one (I-17) (2 g, 7.99 mmol), 5-(2-Bromo-acetyl)-4-methyl-3H-isobenzofuran-1-one (I-4B, method 2, step F) (2.150 g, 7.99 mmol) and N-ethyl-N-isopropylpropan-2-amine (3.48 mL, 19.98 mmol) in DCM (50 mL) were stirred overnight at rt. The mixture was washed with saturated ammonium chloride aqueous and brine, dried over MgSO4, and concentrated under reduced pressure. The crude material was used in the next step without further purification. 1H-NMR (500 MHz, CDCl3): δ ppm 7.83 (1H, d, J=7.8 Hz), 7.79 (1H. d, J=7.8 Hz), 5.34 (2H, s), 5.32 (2H, s), 5.26 (2H, s), 4.03 (2H, t, J=7.0 Hz), 3.71 (1H, m), 3.15 (1H, m), 2.94 (2H, m), 2.47 (2H, t, J=7.0 Hz), 2.42 (3H, s), 2.17 (2H, m), 2.07 (3H, s), 2.02 (2H, m), 1.58 (2H, m). LCMS 438.9 (M+1).

1. washThe mixture was washed with saturated ammonium chloride aqueous and brine
2. dry with materialdried over MgSO4
3. concentrationconcentrated under reduced pressure
4. customThe crude material was used in the next step without further purification