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Ethanol → Ethyl 6-chloronicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 6-Chloronicotinic acid | HCID 79222 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 6-chloronicotinate | HCID 2799611 | — |
反応手順
A mixture of 15.75 g (0.1 mol) 6-chloronicotinic acid, 6.9 g (0.15 mol) ethanol, 22.7 g (0.11 mol) dicyclohexylcarbodiimide and 3.7 g 0.03 mol) dimethylaminopyridine in 200 ml methylene chloride was heated at reflux for 2 hours. The mixture was allowed to cool, solvent removed in vacuo and residue subjected to flash chromatography to give the title compound as a low-melting white solid. PMR (CDCl3): δ1.44 (3 H, t, J~6.2 Hz) 4.44 (2 H, q, J~6.2 Hz), 7.44 (1 H, d, J~8.1 Hz), 8.27 (1 H, dd, J~8.1 Hz, 3 Hz), 9 02 (1 H, d, J3 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246962 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-7d6fedb6c5194b37b83c946407de6f1b |
| 出典メモ | uspto-grants-1993_09 |