تفاعل #439741

معادلة التفاعل

hexane ethyl acetate

compounds 1

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

3,4-dibromothiophene

chloroacetyl chloride

→

2-Chloro-1-(3,4-dibromo- thiophen-2-yl)-ethanone

المردود 97.0%

المذيبات

acetonitrile H2O

ظروف التفاعل

الإجراء التجريبي

General procedure described for compounds 1 and 2 starting from 3,4-dibromothiophene and chloroacetyl chloride. The product was isolated by column chromatography column (hexane:ethyl acetate 8:1). Yield 97%, m.p.: 86-8° C., 1H-NMR (CDCl3): δ7.7 (s, 1H, Ar), 4.8 (s, 2H, CH2); 13C-NMR (CDCl3): δ185.4 (CO), 140.0 (C—CO), 133.7 (CH), 120.8 (C—Br), 119.6 (C—Br), 50.1 (CH2); M/z (EI): 322, 320, 318, 316 (M+, 3, 11, 15, 7%), 271, 269, 267 (M-CH2Cl, 56, 100, 56%); HPLC: Delta Pak Column C18, 5 μm, 300 A, (150×3.9 mm), Purity 94%, r.t.=6.06 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50.

المصدر