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Chloroacetyl chloride → 2-Chloro-1-(3,4-dibromothiophen-2-yl)ethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | 3,4-Dibromothiophene | HCID 18452 | — |
| 反応物 | Chloromethyl Thienyl Ketone deriv. 5 | HCID 6539169 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | 2-Chloro-1-(3,4-dibromothiophen-2-yl)ethan-1-one | HCID 2764204 | 97% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747057B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-cd57abf33d5447bdb3a9f124a5b92606 |
| 出典メモ | uspto-grants-2004_06 |