反应详情

The compound of Example 86 (5.0 g, 10.4 mmol) and imidazole (1.06 g, 15.6 mmol, 1.5 eq.) were dissolved in dichloromethane. tert-Butyldimethylsilylchloride (2.03 g, 13.5 mmol, 1,3 eq.) was added, and the mixture was stirred for 15 hours. Solids were removed by filtration, and the filtrate was concentrated in vacuo. The resulting oil was purified by flash chromatography on silica gel eluted with 90:10 hexanes/ethyl acetate. The title compound was obtained as a yellow oil (5.3 g, 85%): 1H NMR (300 MHz, CDCl3) δ7.30-7.26 (m, 5 H), 7.25-7.20 (m, 3 H), 7.09 (s, 1 H), 6.91 (t, 1 H), 6.80 (d, 2 H), 6.63 (d, 1 H), 4.07-4.00 (m, 2 H), 3.81 (s, 2 H), 3.73 (dd, 1 H), 2.88-2.77 (m, 2 H), 2.64-2.56 (m, 4 H), 1.96-1.90 (m, 1 H), 1.61-1.55 (m, 1 H), 0.85 (s, 9 H), 0.07 (s, 3 H), 0.04 (s, 3 H); MS m/z 596.3 (MH+).

1. customSolids were removed by filtration
2. concentrationthe filtrate was concentrated in vacuo
3. customThe resulting oil was purified by flash chromatography on silica gel
4. washeluted with 90:10 hexanes/ethyl acetate