反应详情

To a solution of (3,5-bis-methoxymethoxy-phenyl)-methanol (220b) (290 g, 1.27 mol) and imidazole (129 g, 1.9 mol) in CH2Cl2 (1.5 L) was added TBSCl (286 g, 1.9 mol) at 5° C. in several portion was stirred at room temperature overnight. TLC (EtOAc/petroleum ether=1/2) showed that the reaction was complete. The mixture was filtered and the filtrate was washed with water, dried over Na2SO4 and concentrated under high vacuum to give the title compound (320 g, 97%) as a brown oil. 1H NMR (400 MHz, CDCl3): δ 6.68 (d, 2H), 6.57(t, 1H), 5.14 (s, 4H), 4.66 (s, 2H), 3.48 (s, 6H), 0.94 (s, 9H), 0.07 (s, 6H).

1. filtrationThe mixture was filtered
2. washthe filtrate was washed with water
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under high vacuum