反应详情

The product from Example 59B (1.37 g, 6 mmol) was suspended in CH2Cl2 (100 mL), treated with TsCl (2.28 g, 12 mmol), treated with 4-dimethylaminopyridine (100 mg, 0.82 mmol), treated with triethylamine (2.2 mL. 16 mmol), and heated at reflux for 4 hours. The mixture was washed with H2O, dried (MgSO4), concentrated under reduced pressure and chromatographed on silica gel eluting with EtOAc:hexanes (25:75) to provide the title compound. 1H NMR (DMSO-d6) δ 1.99 (t, J=6.95 Hz, 2H), 2.23 (t, J=6.95 Hz, 2H), 2.45 (s, 3H), 2.47 (m, 2H), 6.91 (bs, 2H), 7.31 (m, 1H), 7.4 (m, 2H), 7.55 (dd, J=7.29, 1.87 Hz, 1H), 7.5 (d, J=8.48 Hz, 2H), 8.03 (d, J=8.14 Hz, 2H). MS (M+H)+ m/z 382.

1. temperatureheated
2. temperatureat reflux for 4 hours
3. washThe mixture was washed with H2O
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customchromatographed on silica gel eluting with EtOAc:hexanes (25:75)