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Ethyl (chloroformyl)acetate → Ethyl thiazole-5-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl (chloroformyl)acetate | HCID 118030 | — |
| 反応物 | Methanethioamide | HCID 3005587 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Ethyl thiazole-5-carboxylate | HCID 459108 | 60% |
反応手順
To a round bottom flask was added 250 mL of dry acetone, 7.5 g (0.123 mol) of thioformamide, and 18.54 g (0.123 mol) of ethyl 2-chloro-2-formylacetate. The reaction was heated at reflux for 2 hours. The solvent was removed in vacuo, and the residue was purified by chromatography (SiO2, 6 cm o.d. column, 100% CHCl3, Rf =0.25) to provide 11.6 g (60%) of the desired compound as a light yellow oil. NMR (CDCl3) δ1.39 (t, J=7 Hz, 3H), 4.38 (q, J=7 Hz, 2H), 8.50 (s, 1H), 8.95 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05597928 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-44f70e42d0264fd79a876b52447a3202 |
| 出典メモ | uspto-grants-1997_01 |