反应详情

A solution of 103e (3 g, 14.5 mmol), 2,6-dibromo-4-fluorobenzyl acetate 101j (14 g, 43.5 mmol), Xantphos (839 mg, 1.45 mmol), Pd2(dba)3 (1.33 g, 1.45 mmol) and Cs2CO3 (9.4 g, 29 mmol) in dioxane (200 mL) was heated at 100° for 15 h under nitrogen. After filtration, the filtrate was evaporated in vacuo and purified by flash column eluting with ethyl acetate/petroleum ether (1:1) to give 103f (5 g, yield 77%) as a yellow solid. LCMS: (M+H)+452. 1H NMR (500 MHz, DMSO) δ 7.71 (dd, J=2.5, 1H), 7.51 (dd, J=3, 1H), 5.04 (m, 1H), 4.10 (m, 1H), 3.68 (m, 1H), 2.86 (m, 2H), 2.77 (m, 2H), 2.55 (m, 3H), 1.98 (s, 3H), 1.78 (m, 4H)

1. filtrationAfter filtration
2. customthe filtrate was evaporated in vacuo
3. custompurified by flash column
4. washeluting with ethyl acetate/petroleum ether (1:1)