反应详情

General procedure described for compounds 1 and 2 starting from 2,5-dichlorothiophene and chloroacetyl chloride. Purified by column chromatography column (hexane:ethyl acetate 12:1), yield 91%, m.p.: 43-44° C. (ethanol), 1H-NMR (CDCl3): δ7.1 (s, 1H, CH-Aromat), 4.6 (s, 2H, CH2); 13C-NMR (CDCl3): 186.6 (CO), 136.9 (C—Cl), 136.0 (C—CO), 130.2 (C—Cl), 129.4 (CH—Ar), 50.6 (CH2); M/z (EI): 234, 232, 230, 228 (M+, 1, 6, 16, 16%), 183, 181, 179 (M-CH2Cl, 18, 79, 100%), 155, 153, 151 (M-COCH2Cl, 3, 13, 19%), 118, 116 (M-COCH2Cl2, 5, 13%); HPLC: Delta Pak Column C18, 5 μm, 300 A, (150×3.9 mm), Purity 99%, r.t.=6.16 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50.

1. customPurified by column chromatography column (hexane:ethyl acetate 12:1), yield 91%, m.p.: 43-44° C. (ethanol), 1H-NMR (CDCl3): δ7.1 (s, 1H, CH-Aromat), 4.6 (s, 2H, CH2)
2. customDelta Pak Column C18, 5 μm, 300 A, (150×3.9 mm), Purity 99%, r.t.=6.16 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50