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Diisopropyl Ether → 4,5-Diacetoxy-2-pyridinecarbonyl chloride hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 4,5-Diacetoxy-2-pyridinecarboxylic acid | HCID 15077305 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4,5-Diacetoxy-2-pyridinecarbonyl chloride hydrochloride | HCID 22398960 | 158.5% |
反応手順
To a suspension of phosphorus pentachloride (4.6 g) in methylene chloride (40 ml) was added 4,5-diacetoxy-2-pyridinecarboxylic acid (4.5 g) at -20° C. with stirring. The stirring was continued for an hour at -18°~12° C. To the reaction mixture was added diisopropyl ether (80 ml) below 0° C. The resulting precipitates were collected by filtration, washed with diisopropyl ether and dried over phosphorus pentoxide to give 4,5-diacetoxy-2-pyridinecarbonyl chloride hydrochloride (5.15 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05244890 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-2ef62d98fe1447439390fdc1af915ab7 |
| 出典メモ | uspto-grants-1993_09 |