反応 #439746

反応方程式

compounds 1

1-(2-Bromo-4,5-dichloro-thiophen-3-yl)-2-chloro-ethanone

1,2-dibromobenzene

bromoacetyl bromide

→

2-Bromo-1-(3,4-dibromo-phenyl)-ethanone

収率 13.0%

反応条件

後処理

1. 1
   その他Purified by column chromatography column (hexane:ethyl acetate 6:1), yield 13% m.p. 60-61° C., 1H-NMR (CDCl3): δ8.2 (s, 1H, Ar), 7.8 (d, 2H, Ar), 4.4 (s, 2H, CH2)
2. 2
   その他Column μ Bondapack C18, 5 μm, 300 A, (300×3.9 mm), Purity 98%, r.t.=8.73 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50

実験手順

General procedure described for compounds 1 and 2 starting from 1,2-dibromobenzene and bromoacetyl bromide. Purified by column chromatography column (hexane:ethyl acetate 6:1), yield 13% m.p. 60-61° C., 1H-NMR (CDCl3): δ8.2 (s, 1H, Ar), 7.8 (d, 2H, Ar), 4.4 (s, 2H, CH2); 13C-NMR (CDCl3): δ189.7 (CO), 134.6 (CH), 134.4 (CH), 134.3 (C—CO), 132.0 (C—Br), 128.8(CH), 126.2 (C—Br), 30.4 (CH2); M/z (EI): 360, 358, 356, 354 (M+, 5, 14, 14, 5%), 265, 263, 261 (M-CH2Br, 62, 100, 65%); HPLC: Column μ Bondapack C18, 5 μm, 300 A, (300×3.9 mm), Purity 98%, r.t.=8.73 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50.

出典