反应详情

Alkylation of 4-iodophenol with iodide 165 (see Example 2GGG) and K2CO3 as in Example 2GGG above for 6 h, followed by chromatography of the product on silica gel, eluting with petroleum ether (foreruns) and then with 5% CH2Cl2/petroleum ether, gave tert-butyl({2-[(4-iodophenoxy)methyl]-2-propenyl}oxy)dimethylsilane (167) (94%) as an oil; 1H NMR (CDCl3) δ 7.54 (dt, J=8.9, 2.7 Hz, 2H), 6.70 (dt, J=8.9, 2.7 Hz, 2H), 5.25 (d, J=1.0 Hz, 1H), 5.19 (d, J=1.2 Hz, 1H), 4.51 (s, 2H), 4.23 (s, 2H), 0.91 (s, 9H), 0.07 (2 s, 6H); HRFABMS calcd for C16H26H26Si m/z [M+H]+ 405.0747. found 405.0739.

1. customabove for 6 h
2. washeluting with petroleum ether (foreruns)