反应详情

General procedure described for compounds 1 and 2 starting from 1,3,5-tribromobenzene and bromoacetyl bromide. Purified by column chromatography column (hexane:ethyl acetate 6:1), yield 45% m.p.: 86-87° C., 1H-NMR (CDCl3): δ7.7 (s, 2H, Ar), 4.44 (s, 2H, CH2); 13C-NMR (CDCl3): δ193.4 (CO), 139.4 (C—CO), 134.5 (CH), 124.7 (C—Br), 119.4 (C—Br), 34.6 (CH2); M/z (EI): 440, 438, 436, 434, 432 (M+, 1, 3, 5, 3, 1%), 345, 343, 341, 339 (M-CH2Br, 35, 96, 100, 41%); HPLC: Column μ Bondapack C18, 5 μm, 300 A, (300×3.9 mm), Purity 98%, r.t.=3.40 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50.

1. customPurified by column chromatography column (hexane:ethyl acetate 6:1), yield 45% m.p.: 86-87° C., 1H-NMR (CDCl3): δ7.7 (s, 2H, Ar), 4.44 (s, 2H, CH2)
2. customColumn μ Bondapack C18, 5 μm, 300 A, (300×3.9 mm), Purity 98%, r.t.=3.40 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50