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Hydrochloric Acid → 3H-1,2-dihydro-1-pyrrolizinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 3-(Pyrrol-1-yl)propiononitrile | HCID 96527 | — |
| 生成物 | 3H-1,2-dihydro-1-pyrrolizinone | HCID 97347 | 65% |
反応手順
To a solution of 10 g N-cyanoethylpyrrole in 100 ml ether was added 2.5 g ZnCI2. Dried HCl was passed into the mixture at 5°-10° C. After 2 hours, the reaction mixture was allowed to stand at room temperature for 4 hours. Removed the solvent by suction, 20%. Aqueous NaOH was added until pH 3. The mixture was stirred at 80°-90° C. for 2 hours. Extracted with methylene chloride, dried over Na2SO4, evaporated the solvent, 8 g yellow solid was obtained. The crude product was crystallized from petroleum ether, 6.5 g compound (1) was obtained, as white crystals, mp 53°-54.5° C., yield 65%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05616604 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-4e56c64ca6304ac28913658aab4ebe4a |
| 出典メモ | uspto-grants-1997_04 |