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Chloroacetyl chloride → 1-(4-Acetylthiophen-2-yl)-2-chloroethan-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 | 1-(Thiophen-3-yl)ethanone | HCID 15116 | — |
| 反応物 | Chloromethyl Thienyl Ketone deriv. 5 | HCID 6539169 | — |
| 生成物 | 1-(4-Acetylthiophen-2-yl)-2-chloroethan-1-one | HCID 6539172 | 41% |
反応手順
General procedure described for compounds 1 and 2 starting from 3-acetylthiophene and chloroacetyl chloride. Purified by column chromatography column (hexane:ethyl acetate 2:1), yield 41% m.p.: 118-119° C., 1H-NMR (CDCl3): δ8.3 (s, 1H, Ar), 8.1 (s, 1H, Ar), 4.60 (s, 2H, CH2), 2.56 (s, 3H, CH3); 13C-NMR (CDCl3): δ191.6 (CO), 184.5 (CO), 143.3 (C—CO), 141.7 (C—CO), 139.7 (CH), 132.0 (CH), 45.4 (CH2), 27.4 (CH3); M/z (EI): 204, 202 (M+, 6, 17%), 153 (M-CH2Cl, 100%); HPLC: Delta Pak Column C18, 5 μm, 300 A, (150×3.9 mm), Purity 94%, r.t.=2.70 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-e12dad228d3a49ed9f370461e04a848c |
| 出典メモ | uspto-grants-2004_06 |